CN112077298A - ErFe @ GO composite microwave absorbent and preparation method thereof - Google Patents

ErFe @ GO composite microwave absorbent and preparation method thereof Download PDF

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CN112077298A
CN112077298A CN202010842344.2A CN202010842344A CN112077298A CN 112077298 A CN112077298 A CN 112077298A CN 202010842344 A CN202010842344 A CN 202010842344A CN 112077298 A CN112077298 A CN 112077298A
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iron alloy
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graphene oxide
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刘星
庞惠静
傅仁胜
蒙成昆
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Hezhou University
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    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
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Abstract

The invention discloses a rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent and a preparation method thereof, wherein the absorbent comprises 25-50% of graphene oxide powder GO and 50-75% of erbium-iron alloy powder ErFe in percentage by mass, and the mass fraction of Er in the erbium-iron alloy powder is 13%. The preparation process comprises the following steps: er and Fe metal powder with the purity of more than or equal to 99.9 percent is used as a raw material, high-energy ball milling is adopted to prepare rare earth erbium-iron alloy powder, then the erbium-iron powder obtained by ball milling is subjected to vacuum heat treatment, and finally, the ErFe @ GO composite microwave absorbent is prepared by ultrasonic-assisted mechanical stirring. In the 8-18 GHz wave band, a good thin layer broadband strong absorption effect is realized, when the coating thickness is 1.08mm, the minimum reflection loss peak value of the microwave can reach about-42.7 dB, and the corrosion resistance is good.

Description

ErFe @ GO composite microwave absorbent and preparation method thereof
Technical Field
The invention belongs to the field of magnetic composite microwave absorbing materials, and particularly relates to a rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent and a preparation method thereof.
Background
With the popularization of digital equipment and the rapid development of radar detection technology, great convenience is brought to our lives. However, the extensive use of these digital devices and radar detection techniques also generates a large amount of electromagnetic waves into human living spaces, resulting in serious electromagnetic radiation and interference problems, which not only cause damage to highly sensitive electronic devices, but also have significant negative effects on physical health, and have attracted widespread social attention. In order to solve the problems caused by electromagnetic wave radiation, scientists have made a great deal of research work, wherein the microwave absorbing material is used to convert the incident electromagnetic wave energy into other forms of energy, so as to inhibit the radiation and interference of the electromagnetic wave, and have better effect; the method has huge application markets in the civil fields of mobile phones, computers, microwave darkrooms and the like and the military fields of stealth airplanes, radars and the like.
For the research of microwave absorption materials, the formula design and preparation technology of the absorbent are the key points of the research of the microwave absorption materials. At present, two main types of common microwave absorbers include electrically lossy absorbers and magnetically lossy absorbers. The electrically lossy absorbents mainly include carbon-based absorbents and ceramic-based absorbents; the magnetic loss type absorbent mainly comprises Fe, Co and Ni simple substances, alloy, oxides thereof and the like. The rare earth elements have special electric, magnetic, optical and catalytic performances and are known as treasury designed by new materials. A certain amount of rare earth elements are added into the iron-based alloy to prepare the rare earth iron-based alloy absorbent, so that the physical property and the microwave absorption property of the iron-based alloy can be better improved. The graphene oxide surface has a plurality of suspended chemical bonds, so that more polarization loss mechanisms can be provided; the electrical resistivity is high, the eddy current effect of metal can be regulated and controlled, and the physical properties are excellent.
However, among the existing many absorbents, it is difficult for a single-component absorbent to simultaneously satisfy the requirements of thin thickness, low density, wide frequency band, strong absorption, excellent physical properties, etc., and especially for a thin-layer wave-absorbing material with small thickness, it is more difficult to achieve the requirements of a "thin, light, strong, wide" high-performance wave-absorbing material. The composite absorbent can overcome the defect of single component, can exert the respective characteristics of each material, realizes the good and bad complementation by utilizing the complementarity of the electromagnetic characteristics, different loss mechanisms and component proportion of the materials, finally obtains the effect of adding one to more than two, and is the development way of the future wave-absorbing material.
Disclosure of Invention
The invention aims to solve the problems that the existing single-component absorbent is difficult to realize strong absorption, wide frequency band, light weight and excellent physical properties of a wave-absorbing material when the thickness is thin, and provides a rare earth erbium-iron alloy-graphene oxide composite microwave absorbent which has strong absorption, wide frequency band, good thermal stability, certain oxidation resistance and corrosion resistance in a microwave band of 8-18 GHz when the thickness is thin.
The invention aims to provide a rare earth erbium iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent, which comprises 50-75% of rare earth erbium iron alloy powder ErFe and 25-50% of graphene oxide powder GO by mass percentage, wherein Er accounts for 13% of the mass fraction of the erbium iron alloy powder.
The invention also aims to provide a preparation method of the rare earth erbium-iron-based alloy-graphene oxide composite microwave absorbent.
The preparation method of the rare earth erbium-iron alloy-graphene oxide composite microwave absorbent comprises the following main steps:
(1) preparing materials: er and Fe metal powder with the purity of more than or equal to 99.9 percent is used as a raw material, and Er iron powder is prepared according to the mass percent of Er to Fe which is 13 to 87;
(2) high-energy ball milling: preparing rare earth erbium-iron alloy powder from erbium iron powder by adopting high-energy ball milling;
(3) vacuum heat treatment: carrying out vacuum heat treatment on the rare earth erbium-iron alloy powder;
(4) ultrasonic auxiliary mechanical stirring: and (3) preparing the rare earth erbium-iron alloy-graphene oxide composite microwave absorbent by ultrasonic-assisted mechanical stirring.
The main process of the high-energy ball milling in the step (2) is that stainless steel balls and pure erbium iron powder are placed into a stainless steel tank according to the mass ratio of 20:1, ball milling is carried out for 70 hours under the condition that cyclohexane, absolute ethyl alcohol or gasoline is used as a grinding aid, and the rotating speed of a ball mill is 350 r/min.
And (3) putting the rare earth erbium-iron alloy powder into a vacuum heat treatment furnace, vacuumizing, washing with argon for 3-5 times, heating to 400-500 ℃ at a heating rate of 5-15 ℃/min, preserving heat for 2-4 h, and cooling along with the furnace.
Dispersing weighed graphene oxide powder in absolute ethyl alcohol, and performing ultrasonic treatment for 15-20 min at 100w power; and (4) adding the rare earth erbium-iron alloy powder obtained in the step (3) into an absolute ethyl alcohol system according to a certain ratio, simultaneously starting ultrasonic oscillation and mechanical stirring at the stirring speed of 30-50 r/min until the solution is completely volatilized, and drying to obtain the rare earth erbium-iron alloy-graphene oxide composite microwave absorbent.
The method for detecting the electromagnetic parameters and the reflection loss RL of the product comprises the following steps: mixing the rare earth erbium-iron alloy-graphene oxide composite microwave absorbent and paraffin wax in a ratio of 40:60 (mass ratio) to prepare coaxial samples with the outer diameter and the inner diameter of 7mm and 3mm respectively and the thickness of 2.0-3.0 mm, and measuring the complex dielectric constant and the complex permeability of the samples in a frequency range of 8-18 GHz by using a microwave vector network analyzer. And then simulating the reflection loss RL of the single-layer wave-absorbing material under the thickness of 1.0-1.3 mm by adopting the following formula.
RL=20lg|(Zin-Z0)/(Zin+Z0)|
Figure BDA0002641898240000031
Wherein Z isinIs the input impedance, Z, of the wave-absorbing material0The free space impedance is 377 omega, f is the frequency of incident electromagnetic wave, d is the thickness of the wave-absorbing material, c is the propagation speed of light in vacuum,rand murThe measured complex permittivity and complex permeability, respectively, j being an imaginary unit.
Experiments prove that in a wave band of 8-18 GHz, when the thickness of the wave-absorbing coating changes within 1.15-1.30 mm, the minimum value of the reflection loss of the compound to microwaves is less than-10 dB (90% of electromagnetic waves are absorbed), so that a good thin-layer broadband strong absorption effect is realized, the position of an absorption peak of the composite absorption material can be conveniently adjusted according to the thickness of the coating, and more than 90% of electromagnetic waves with different frequencies are absorbed. When the coating thickness of the ErFe @ GO composite absorbent is 1.08mm, the minimum reflection loss peak value of the ErFe @ GO composite absorbent for microwaves can reach about-42.7 dB, and the ErFe @ GO composite absorbent has a good broadband effect and has application potential as a high-performance thin-layer wave-absorbing material.
The rare earth erbium-iron alloy-graphene oxide composite microwave absorbent has good microwave absorption characteristic in a microwave band of 8-18 GHz, and has the characteristics of thin thickness, strong absorption, wide frequency band, good temperature stability, good corrosion resistance, simple preparation process and the like. The erbium-iron alloy-graphene oxide wave absorber is suitable for preparing microwave absorption products with thin thickness, wide absorption frequency band, good wave absorption performance, good thermal stability, certain oxidation resistance and corrosion resistance.
Drawings
FIG. 1 is a process flow diagram of a preparation method of the present invention;
fig. 2 is a graph showing the reflection loss of 50:50 wt% rare earth erbium iron alloy-graphene oxide (ErFe @ GO) composite microwave absorber (d ═ 1.0mm, 1.08mm, 1.15mm, 1.2mm, 1.25mm, 1.3mm) as a function of frequency;
fig. 3 is a graph showing the results of the relationship between the reflection loss and the frequency of a rare earth erbium iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent (d ═ 1.0mm, 1.08mm, 1.15mm, 1.2mm, 1.25mm, 1.3mm) with a mass ratio of 70: 30;
fig. 4 is a graph showing the relationship between reflection loss and frequency of a rare earth erbium iron alloy-graphene oxide (ErFe @ GO) composite microwave absorber (d ═ 1.0mm, 1.08mm, 1.15mm, 1.2mm, 1.25mm, 1.3mm) at a mass ratio of 75: 25;
fig. 5 is a graph showing the results of the relationship between reflection loss and frequency of the rare earth erbium iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbers with different mass percentages (25:75, 50:50, 70:30, 75:25, 80:20) under the condition that d is 1.15 mm.
Detailed Description
Example 1:
the specific implementation steps for preparing the rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent with the mass percentage of 50:50 are as follows:
1) er and Fe metal powder with the purity of more than or equal to 99.9 percent is used as a raw material, and Er iron powder is prepared according to the mass percent of Er to Fe which is 13 to 87;
2) putting a stainless steel ball and weighed erbium iron powder into a stainless steel tank according to the mass ratio of 20:1, ball-milling for 70 hours by adopting a high-energy ball mill under the condition that cyclohexane is taken as a grinding aid, wherein the rotating speed of the ball mill is 350r/min, cleaning by using absolute ethyl alcohol, drying and ball-milling to obtain a sample, and obtaining rare earth erbium iron alloy powder;
3) putting the rare earth erbium-iron alloy powder into a vacuum heat treatment furnace, vacuumizing, washing with argon gas for 3 times, heating to 400 ℃ at a heating rate of 5 ℃/min, preserving heat for 4 hours, and cooling along with the furnace;
4) weighing the rare earth erbium-iron alloy powder and the graphene oxide powder which are subjected to vacuum heat treatment according to the mass percentage of 50: 50; firstly, carrying out ultrasonic treatment on weighed graphene oxide powder for 15min under the power of 100w, and uniformly dispersing the graphene oxide powder in absolute ethyl alcohol; and then pouring the proportioned erbium-iron alloy powder into absolute ethyl alcohol, simultaneously starting ultrasonic oscillation and mechanical stirring at the stirring speed of 30r/min, and drying until the solution is volatilized completely to obtain the rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent.
And (3) product testing: mixing the ErFe @ GO absorbent and paraffin wax in a ratio of 40:60 (mass ratio) to prepare coaxial samples with outer diameters and inner diameters of 7mm and 3mm respectively and thicknesses of 2.0-3.0 mm, and respectively measuring complex permeability and complex dielectric constant of the samples in a frequency band of 8-18 GHz by using a microwave vector network analyzer. Then, the reflection loss RL of the single-layer wave-absorbing material at the thicknesses of 1.15mm, 1.2mm, 1.25mm and 1.3mm is simulated by adopting the following formula calculation.
RL=20lg|(Zin-Z0)/(Zin+Z0)|
Figure BDA0002641898240000051
Wherein Z isinIs the input impedance, Z, of the wave-absorbing material0The free space impedance is 377 omega, f is the frequency of incident electromagnetic wave, d is the thickness of the wave-absorbing material, c is the propagation speed of light in vacuum,rand murThe measured complex permittivity and complex permeability, respectively, j being an imaginary unit.
Performance test results and analysis:
FIG. 2 shows the reflection loss RL of ErFe @ GO absorbent with the mass percentage of 50:50 and the thicknesses of 1.15mm, 1.2mm, 1.25mm and 1.3mm in the 8-18 GHz microwave band respectively. From the figure, it can be seen that: in all the thicknesses, the absorption peak value of the composite is less than-10 dB (the absorption rate is more than 90%), the composite has better microwave absorption characteristic and better broadband effect; when the thickness of the compound is 1.25mm, the minimum reflectivity peak value at the frequency of 17.8GHz reaches about-17.4 dB, and the compound has application potential of becoming a high-performance thin-layer light wave-absorbing material.
Example 2
The specific implementation steps for preparing the rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent with the mass percentage of 70:30 are as follows:
1) er and Fe metal powder with the purity of more than or equal to 99.9 percent is used as a raw material, and Er iron powder is prepared according to the mass percent of Er to Fe which is 13 to 87;
2) putting a stainless steel ball and weighed erbium iron powder into a stainless steel tank according to the mass ratio of 20:1, ball-milling for 70 hours by adopting a high-energy ball mill under the condition that absolute ethyl alcohol is used as a grinding aid, wherein the rotating speed of the ball mill is 350r/min, cleaning by using the absolute ethyl alcohol, drying and ball-milling to obtain a sample, and thus obtaining the rare earth erbium iron alloy powder.
3) Putting the rare earth erbium-iron alloy powder into a vacuum heat treatment furnace, vacuumizing, washing with argon for 5 times, heating to 450 ℃ at a heating rate of 10 ℃/min, preserving heat for 3 hours, and cooling along with the furnace;
4) weighing the rare earth erbium-iron alloy powder and the graphene oxide powder which are subjected to vacuum heat treatment according to the mass percentage of 70: 30; firstly, carrying out ultrasonic treatment on weighed graphene oxide powder for 20min under the power of 100w, and uniformly dispersing the graphene oxide powder in absolute ethyl alcohol; and then pouring the proportioned erbium-iron alloy powder into absolute ethyl alcohol, simultaneously starting ultrasonic oscillation and mechanical stirring at the stirring speed of 40r/min, and drying until the solution is volatilized completely to obtain the rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent.
And (3) product testing: coaxial samples with an outer diameter and an inner diameter of 7mm and 3mm, respectively, and a thickness of about 2.0 to 3.0mm were prepared by mixing an ErFe @ GO absorbent and paraffin wax at a ratio of 40:60 (mass ratio), and reflection losses RL of 1.0mm, 1.10mm, 1.15mm, 1.2mm, 1.25mm, and 1.3mm, respectively, were simulated using a computer program as in example 1.
Performance test results and analysis:
FIG. 3 shows the reflection loss RL of ErFe @ GO absorbent with the mass percentage of 70:30 and the thicknesses of 1.0mm, 1.10mm, 1.15mm, 1.2mm, 1.25mm and 1.3mm in a microwave band of 8-18 GHz respectively. From the figure, it can be seen that: in all the thicknesses, the absorption peak value of the composite is less than-10 dB (the absorption rate is more than 90%), the composite has better microwave absorption characteristic and better broadband effect; when the thickness of the compound is 1.10mm, the minimum reflectivity peak value at the frequency of 16.7GHz reaches about-18.3 dB, the frequency bandwidth (< -10dB) reaches 3GHz, and the compound has the application potential of becoming a high-performance thin-layer broadband wave-absorbing material.
Example 3:
the specific implementation steps for preparing the rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent with the mass percent of 75:25 are as follows:
1) er and Fe metal powder with the purity of more than or equal to 99.9 percent is used as a raw material, and Er iron powder is prepared according to the mass percent of Er to Fe which is 13 to 87;
2) putting a stainless steel ball and weighed erbium iron powder into a stainless steel tank according to the mass ratio of 20:1, ball-milling for 70 hours by adopting a high-energy ball mill under the condition that gasoline is taken as a grinding aid, wherein the rotating speed of the ball mill is 350r/min, cleaning by using absolute ethyl alcohol, drying and ball-milling to obtain a sample, and obtaining the rare earth erbium iron alloy powder.
3) Putting the rare earth erbium-iron alloy powder into a vacuum heat treatment furnace, vacuumizing, washing gas for 4 times by argon, then heating to 500 ℃ at a heating rate of 15 ℃/min, preserving heat for 2 hours, and then cooling along with the furnace;
4) weighing the rare earth erbium-iron alloy powder and the graphene oxide powder which are subjected to vacuum heat treatment according to the mass percentage of 75: 25; firstly, carrying out ultrasonic treatment on weighed graphene oxide powder for 20min under the power of 100w, and uniformly dispersing the graphene oxide powder in absolute ethyl alcohol; and then pouring the proportioned erbium-iron alloy powder into absolute ethyl alcohol, simultaneously starting ultrasonic oscillation and mechanical stirring at a stirring speed of 50r/min, and drying until the solution is volatilized completely to obtain the rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent.
And (3) product testing: coaxial samples with an outer diameter and an inner diameter of 7mm and 3mm respectively and a thickness of about 2.0-3.0 mm were prepared by mixing the ErFe @ GO alloy powder and paraffin wax at a ratio of 40:60 (mass ratio), and reflection losses RL with thicknesses of 1.0mm, 1.08mm, 1.15mm, 1.2mm, 1.25mm, and 1.3mm were simulated by using a computer program as in example 1.
Performance test results and analysis:
FIG. 4 shows the reflection loss RL of ErFe @ GO absorbent with the mass percentage of 75:25, respectively with the thickness of 1.0mm, 1.08mm, 1.15mm, 1.2mm, 1.25mm and 1.3mm in the microwave band of 8-18 GHz. From the figure, it can be seen that: in all the thicknesses, the absorption peak value of the composite is less than-10 dB (the absorption rate is more than 90%), and the position of the minimum absorption peak can be conveniently adjusted through the thickness of the coating, so that the composite has better microwave absorption characteristic and broadband effect; when the thickness of the compound is 1.08mm, the minimum reflectivity peak value at the frequency of 17.2GHz reaches about-42.7 dB, the frequency bandwidth (< -10dB) reaches 2.6GHz, and the compound has application potential as a high-performance thin-layer broadband wave-absorbing material.
Comparative example:
the specific implementation steps for preparing the rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent with different mass percentages (25:75, 50:50, 70:30, 75:25 and 80:20) are as follows:
1) er and Fe metal powder with the purity of more than or equal to 99.9 percent is used as a raw material, and Er iron powder is prepared according to the mass percent of Er to Fe which is 13 to 87;
2) putting a stainless steel ball and weighed erbium iron powder into a stainless steel tank according to the mass ratio of 20:1, ball-milling for 70 hours by adopting a high-energy ball mill under the condition that gasoline is taken as a grinding aid, wherein the rotating speed of the ball mill is 350r/min, cleaning by using absolute ethyl alcohol, drying and ball-milling to obtain a sample, and obtaining the rare earth erbium iron alloy powder.
3) Putting the rare earth erbium-iron alloy powder into a vacuum heat treatment furnace, vacuumizing, washing gas for 4 times by argon, then heating to 500 ℃ at a heating rate of 15 ℃/min, preserving heat for 2 hours, and then cooling along with the furnace;
4) weighing the rare earth erbium-iron alloy powder and the graphene oxide powder which are subjected to vacuum heat treatment respectively according to the mass percentages of 25:75, 50:50, 70:30, 75:25 and 80: 20; firstly, carrying out ultrasonic treatment on weighed graphene oxide powder for 20min under the power of 100w, and uniformly dispersing the graphene oxide powder in absolute ethyl alcohol; and then pouring the proportioned erbium-iron alloy powder into absolute ethyl alcohol, simultaneously starting ultrasonic oscillation and mechanical stirring at a stirring speed of 50r/min, and drying until the solution is volatilized completely to obtain the rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent.
And (3) product testing: coaxial samples with an outer diameter and an inner diameter of 7mm and 3mm respectively and a thickness of about 2.0 to 3.0mm were prepared by mixing an ErFe @ GO absorbent and paraffin wax of 40:60 (mass ratio), and the reflection loss RL with a thickness of 1.15mm was simulated by using a computer program as in example 1.
Performance test results and analysis:
FIG. 5 shows the reflection loss RL of 1.15mm in thickness in the 8-18 GHz microwave band for ErFe @ GO absorbers of different mass percentages of 25:75, 50:50, 70:30, 75:25, and 80: 20.
From the figure, it can be seen that: among different mass percentages, the ErFe @ GO absorbent with the mass percentages of 50:50, 70:30 and 75:25 can realize-10 dB (the absorptivity is more than 90%) under the thickness of 1.15mm, wherein the best mass percentage is 75:25, the minimum reflectivity peak value reaches about-22.9 dB at the frequency of 16.2GHz, and the frequency bandwidth (< -10dB) reaches 3.9 GHz; however, the ErFe @ GO absorbents with the percentages of 25:75 and 80:20 have poor wave absorbing performance and high minimum reflectivity.
Therefore, after the graphene oxide powder GO with the mass percentage of 25-50% and the erbium iron alloy powder ErFe with the mass percentage of 50-75% are mixed in the range, the wave absorbing performance is better.

Claims (5)

1. A rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent is characterized in that: the powder comprises 50-75% of erbium iron alloy powder ErFe and 25-50% of graphene oxide powder GO by mass percentage, wherein Er in the erbium iron alloy powder accounts for 13% of the mass fraction of the erbium iron alloy powder.
2. A method for preparing the rare earth erbium iron alloy-graphene oxide (ErFe @ GO) composite microwave absorber according to claim 1, comprising the following main steps:
(1) preparing materials: er and Fe metal powder with the purity of more than or equal to 99.9 percent is used as a raw material, and Er iron powder is prepared according to the mass percent of Er to Fe which is 13 to 87;
(2) high-energy ball milling: preparing rare earth erbium-iron alloy powder from erbium iron powder by adopting high-energy ball milling;
(3) vacuum heat treatment: carrying out vacuum heat treatment on the rare earth erbium-iron alloy powder;
(4) ultrasonic auxiliary mechanical stirring: and (3) preparing the rare earth erbium-iron alloy-graphene oxide composite microwave absorbent by ultrasonic-assisted mechanical stirring.
3. The preparation method of the rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent according to claim 2, wherein the main process of the high-energy ball milling in the step (2) is that a stainless steel ball and pure erbium iron powder are put into a stainless steel tank according to the mass ratio of 20:1, and are ball-milled for 70 hours under the condition that cyclohexane, absolute ethyl alcohol or gasoline is used as a grinding aid, and the rotating speed of the ball mill is 350 r/min.
4. The preparation method of the rare earth erbium-iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent according to claim 3, wherein the vacuum heat treatment in the step (3) mainly comprises the steps of putting rare earth erbium-iron alloy powder into a vacuum heat treatment furnace, vacuumizing, washing with argon for 3-5 times, heating to 400-500 ℃ at a heating rate of 5-15 ℃/min, preserving heat for 2-4 hours, and cooling along with the furnace.
5. The preparation method of the rare earth erbium iron alloy-graphene oxide (ErFe @ GO) composite microwave absorbent according to claim 4, wherein the main process of the ultrasonic-assisted mechanical stirring in the step (4) is that weighed graphene oxide powder is dispersed in absolute ethyl alcohol, and the ultrasonic treatment is carried out for 15-20 min under the power of 100 w; and (4) adding the rare earth erbium-iron alloy powder obtained in the step (3) into an absolute ethyl alcohol system according to a certain ratio, simultaneously starting ultrasonic oscillation and mechanical stirring at the stirring speed of 30-50 r/min until the solution is completely volatilized, and drying to obtain the rare earth erbium-iron alloy-graphene oxide composite microwave absorbent.
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CN104388818A (en) * 2014-11-14 2015-03-04 桂林电子科技大学 ErFeV magnetic wave-absorbing material and preparation method thereof
CN105603296A (en) * 2015-12-23 2016-05-25 桂林电子科技大学 Rare earth Fe-based electromagnetic shielding material and preparation method thereof
CN108865060A (en) * 2018-06-04 2018-11-23 中国航发北京航空材料研究院 The preparation method and applications of graphene composite wave-suction material based on 5G communication

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CN112687351A (en) * 2021-01-07 2021-04-20 哈尔滨工业大学 Method for rapidly predicting microwave electromagnetic performance of composite medium based on genetic algorithm-BP neural network

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