CN114309586B - High-entropy alloy/carbon black composite electromagnetic wave-absorbing material and preparation method thereof - Google Patents
High-entropy alloy/carbon black composite electromagnetic wave-absorbing material and preparation method thereof Download PDFInfo
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- 239000006229 carbon black Substances 0.000 title claims abstract description 134
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 132
- 239000000956 alloy Substances 0.000 title claims abstract description 132
- 239000011358 absorbing material Substances 0.000 title claims abstract description 108
- 239000002131 composite material Substances 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 60
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 51
- 229910052751 metal Inorganic materials 0.000 claims abstract description 50
- 239000002184 metal Substances 0.000 claims abstract description 50
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 41
- 229910052742 iron Inorganic materials 0.000 claims abstract description 33
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 26
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 21
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 19
- 239000011651 chromium Substances 0.000 claims abstract description 14
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 14
- 238000000498 ball milling Methods 0.000 claims description 88
- 239000000843 powder Substances 0.000 claims description 68
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- 230000008569 process Effects 0.000 claims description 31
- 238000012216 screening Methods 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000002994 raw material Substances 0.000 claims description 21
- 238000001291 vacuum drying Methods 0.000 claims description 21
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a high-entropy alloy/carbon black composite electromagnetic wave-absorbing material, which is characterized in that the molecular formula of the high-entropy alloy/carbon black is (FeNiCrAl a ) x C y Wherein a is the molar ratio of Al to Fe, ni and Cr, and x and y are FeNiCrAl in the high-entropy alloy/carbon black respectively a The invention combines the quaternary high-entropy alloy composed of Fe, ni, cr and Al and carbon black, has magnetic loss and electric loss, effectively improves the wave absorbing performance of the material, and has the advantages ofThe broadband high-efficiency electromagnetic wave absorbing performance is realized, and the broadband high-efficiency electromagnetic wave absorbing device is widely applied to various civil and military electromagnetic wave absorbing fields; in addition, the invention also provides a preparation method of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material, and the method realizes the preparation of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material by performing high-energy ball milling on metal iron, metal nickel, metal chromium, metal aluminum and carbon black to perform alloying and compounding.
Description
Technical Field
The invention belongs to the technical field of high-entropy alloy composite materials, and particularly relates to a high-entropy alloy/carbon black composite electromagnetic wave-absorbing material and a preparation method thereof.
Background
With the rapid development of the electronic industry, more and more electromagnetic waves fill living space of people, so that a great amount of electromagnetic wave pollution is caused, and the electromagnetic pollution also becomes fourth pollution after air pollution, water pollution and noise pollution. Electromagnetic wave pollution is not only unfavorable for the normal operation of electronic equipment, but also can damage the physical and mental health of human beings. The electromagnetic wave absorbing material can absorb electromagnetic wave pollution in surrounding environment, so that people do not receive the harm of electromagnetic waves, and therefore, the high-efficiency wave absorbing material also becomes a focus of social attention, and has important value in both military and civil fields.
Electromagnetic absorbers play a decisive role in wave absorbing materials, and there are three main types of electromagnetic absorbers: magnetic absorbers, electrically conductive absorbers, and dielectric absorbers. However, the magnetic absorber has the advantages of magnetic disappearance at high temperature, small loss of the conductive absorber and the dielectric absorber and poor absorption capacity, so that a novel wave absorbing material is necessary to be developed.
The high-entropy alloy is a research direction which is developed in recent years and is rapidly growing, and the high-entropy alloy has advantages over the traditional alloy in the aspects of mechanical, physical, chemical and other properties. With the deep research of the high-entropy alloy, the high-entropy alloy is not limited by five-membered equal atomic ratio any more, and the quaternary high-entropy alloy, in particular to the development of the non-equal atomic ratio high-entropy alloy, so that the wave-absorbing material has a larger space in the selection of components. The composition design of the combination of the high-entropy alloy and the carbon substance, namely the combination of the magnetic loss and the electric loss, greatly improves the performance of the wave-absorbing material.
Therefore, a high-entropy alloy/carbon black composite electromagnetic wave-absorbing material and a preparation method thereof are needed.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-entropy alloy/carbon black composite electromagnetic wave-absorbing material aiming at the defects of the prior art. The material is composed of quaternary high-entropy alloy composed of Fe, ni, cr and Al and carbon black in a composite mode, has magnetic loss and electric loss, effectively improves the wave absorbing performance of the material, has broadband high-efficiency electromagnetic wave absorbing performance, and is widely applied to various civil and military electromagnetic wave absorbing fields.
In order to solve the technical problems, the invention adopts the following technical scheme: the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material is characterized in that the molecular formula of the high-entropy alloy/carbon black is (FeNiCrAl a ) x C y Wherein a is the molar ratio of Al to Fe, ni and Cr, and x and y are FeNiCrAl in the high-entropy alloy/carbon black respectively a And mass fraction of C.
The invention uses Fe, ni, cr and Al to compose quaternary high entropy alloy, which has ideal soft magnetic property and satisfies the condition of composing magnetic dielectric loss type wave absorbing material, the invention uses carbon black as the material of electric loss mechanism, and uses FeNiCrAl a The quaternary high-entropy alloy and the carbon black are combined, so that various loss mechanisms can be provided, the wave absorbing performance of the material is improved, and the high-entropy alloy/carbon black composite electromagnetic wave absorbing material with excellent performance is provided.
The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material is characterized in that the a satisfies the following conditions: a is more than or equal to 0.1 and less than or equal to 0.5; the x satisfies the following conditions: x is more than or equal to 90 and less than or equal to 99, and y satisfies the following conditions: 1.ltoreq.y.ltoreq.10, and x+y=100. The invention limits the content of Al in the quaternary high-entropy alloy by controlling the numerical range of a, so that the Al and Ni in the quaternary high-entropy alloy are fully formedNi 2 Al phase is separated out on the matrix, the unordered arrangement improves the resistivity of the alloy, effectively reduces the hysteresis loss of the alloy, provides guarantee for the service of the alloy in a high-temperature environment, leads the magnetic loss in the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material to be dominant by controlling the numerical range of x and y, and ensures that the novel wave-absorbing material of the high-entropy alloy plays the wave-absorbing advantage of the novel wave-absorbing material in the severe environment such as high temperature.
In addition, the invention also provides a method for preparing the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material, which is characterized by comprising the following steps:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material;
step two, adding the raw materials, ethanol and stainless steel grinding balls obtained in the step one into a ball milling tank for stirring, and then sealing the ball milling tank in a glove box filled with argon to obtain a sealed ball milling tank;
step three, mounting the sealed ball milling tank obtained in the step two on a high-energy ball mill for high-energy ball milling, opening the sealed ball milling tank after the high-energy ball milling in a glove box filled with argon, and obtaining precursor powder in the sealed ball milling tank;
and step four, sequentially carrying out vacuum drying and screening on the precursor powder obtained in the step three to obtain the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder.
The invention mixes metal iron, metal nickel, metal chromium, metal aluminum and carbon black and then carries out high-energy ball milling, the metal iron, the metal nickel, the metal chromium and the metal aluminum are alloyed through collision of grinding balls in the ball milling process, and chemical overreaction is carried out, thus forming FeNiCrAl a Quaternary high entropy alloys, carbon black and FeNiCrAl a The quaternary high-entropy alloy is compounded in a physical mode in a high-energy ball milling process to obtain the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material, the energy consumption in the preparation process is low, the cost is low, the operation is simple, the preparation of the high-entropy alloy/composite wave-absorbing material is enabled to be possible, the electromagnetic wave-absorbing performance of the magnetic metal material is improved through alloying and material compounding, and the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material is prepared by using a mechanical alloying methodThe high-entropy alloy/composite wave-absorbing material prepared by the method has excellent wave-absorbing performance and wide application prospect, further expands the application field of the high-entropy alloy and provides a new idea for the development of the high-entropy alloy; according to the invention, ethanol is added in the ball milling process, so that the control agent is used, the alloy is prevented from being oxidized in the high-energy ball milling process, and cold welding blocking in the high-energy ball milling process is prevented, so that the ball-milled powder is dispersed.
The method is characterized in that the mass purity of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black in the first step is more than 99.5 percent; the particle size of the carbon black is less than 1 mu m. The invention controls the quality purity of metal iron, metal nickel, metal chromium, metal aluminum and carbon black, thereby controlling the purity of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material, ensuring the performance of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material.
The method is characterized in that the premixing in the first step is to perform clockwise and anticlockwise alternate grinding for 30 min-60 min in a mortar. According to the invention, through clockwise and anticlockwise alternate grinding, the grinding balls are more fully contacted with the powder, and alloying and material compounding are more uniform, so that the component uniformity of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material is ensured.
The method is characterized in that in the third step, the ball-material ratio in the high-energy ball milling process is 10-20: 1. the invention adopts higher ball-material ratio, so that larger energy is provided in the ball milling process, smooth alloying is ensured, and the preparation of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material is realized.
The method is characterized in that the rotating speed of the high-energy ball milling in the third step is 300 r/min-450 r/min, the ball milling time is 60-90 h, and the high-energy ball milling is stopped for 1-5 min every 30-60 min. The invention ensures the smooth progress of alloying and compounding by controlling the rotating speed, prevents the defects that the alloying process cannot be successfully completed due to the too small rotating speed and the impact force of a grinding ball is too large to cause the damage of a ball milling tank to generate serious scrap iron pollution and influence the component content of the high-entropy alloy wave-absorbing material.
The method is characterized in that the conditions of vacuum drying in the fourth step are as follows: heating to 60-80 ℃ under the condition of 0.8-1 Pa of vacuum degree, and preserving heat for 12h. The invention makes the ethanol in the raw materials fully play a role through vacuum drying, so as to facilitate the test and detection of the following samples.
The method is characterized in that the screening process in the fourth step is as follows: sieving with 100 mesh, 200 mesh and 300 mesh sieve. The invention obtains the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder with the required particle size through screening.
Compared with the prior art, the invention has the following advantages:
1. the invention mixes metal iron, metal nickel, metal chromium, metal aluminum and carbon black and then carries out high-energy ball milling, the metal iron, the metal nickel, the metal chromium and the metal aluminum are alloyed through collision of grinding balls in the ball milling process, and chemical overreaction is carried out, thus forming FeNiCrAl a Quaternary high entropy alloys, carbon black and FeNiCrAl a The quaternary high-entropy alloy is compounded in a physical mode in the high-energy ball milling process to obtain the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material, and the preparation process has the advantages of low energy consumption, low cost and simplicity in operation.
2. The invention improves the electromagnetic wave-absorbing performance of the magnetic metal material through alloying and material compounding, prepares high-entropy alloy powder by using a mechanical alloying method, introduces a large number of crystal defects into the high-entropy alloy powder, and can be used as polarization centers to enhance polarization effects, thereby improving the electromagnetic wave-absorbing performance of the material.
3. According to the invention, ethanol is added in the ball milling process, so that the control agent is used, the alloy is prevented from being oxidized in the high-energy ball milling process, and cold welding blocking in the high-energy ball milling process is prevented, so that the ball-milled powder is dispersed.
4. The method adjusts the atomic percentage of Al element and the mass percentage of carbon black in the radar wave-absorbing coating material, limits the content of Al in the quaternary high-entropy alloy, and ensures that the Al and Ni in the quaternary high-entropy alloy fully form Ni 2 The Al phase is separated out on the matrix, the unordered arrangement improves the resistivity of the alloy, effectively reduces the hysteresis loss of the alloy, provides a guarantee for the service of the alloy in a high-temperature environment, leads the magnetic loss in the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material to be dominant, and ensures that the novel wave-absorbing material of the high-entropy alloy exerts the wave-absorbing advantage of the novel wave-absorbing material in a severe environment such as high temperature.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a graph showing the wave absorbing performance of the high entropy alloy/carbon black composite electromagnetic wave absorbing material prepared in example 1 of the present invention.
FIG. 2 is a graph showing the wave absorbing performance of the high entropy alloy/carbon black composite electromagnetic wave absorbing material prepared in example 2 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material; the mass purity of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black is more than 99.5 percent; the particle size of the carbon black is less than 1 mu m; the premixing is to grind alternately clockwise and anticlockwise in a mortar for 60min, and the alternation of clockwise and anticlockwise is performed every 5min;
step two, adding the raw materials, ethanol and stainless steel grinding balls obtained in the step one into a ball milling tank for stirring, and then sealing the ball milling tank in a glove box filled with argon to obtain a sealed ball milling tank;
step three, mounting the sealed ball milling tank obtained in the step two on a high-energy ball mill for high-energy ball milling, opening the sealed ball milling tank after the high-energy ball milling in a glove box filled with argon, and obtaining precursor powder in the sealed ball milling tank; the ball-material ratio in the high-energy ball milling process is 10:1, a step of; the rotating speed of the high-energy ball milling is 400r/min, the ball milling time is 60h, and the ball milling stays for 3min every 30 min;
step four, sequentially carrying out vacuum drying and screening on the precursor powder obtained in the step three to obtain high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder; the conditions of the vacuum drying are as follows: heating to 70 ℃ under the condition of vacuum degree of 1Pa, and preserving heat for 12 hours; the screening process comprises the following steps: and screening by adopting a 100-mesh filter screen, a 200-mesh filter screen and a 300-mesh filter screen in sequence, wherein the grain size of the high-entropy alloy/carbon black composite electromagnetic wave absorbing material powder is smaller than 5 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is (FeNiCrAl) 0.3 ) 99 C 1 。
The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is mixed with paraffin to prepare a test sample with the inner diameter of 3mm, the outer diameter of 7mm and the thickness of 2mm, and then the test sample is subjected to wave-absorbing performance detection, the maximum reflection loss value of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in the embodiment is-50.91 dB, the corresponding frequency is 5.51GHz, the effective wave-absorbing frequency is 2.36GHz, and meanwhile, the 2.36GHz is the maximum effective wave-absorbing frequency, the maximum reflection loss is smaller than-10 dB required by the wave-absorbing material, so that the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment has excellent wave-absorbing performance.
Fig. 1 is a wave absorbing performance curve of the high-entropy alloy/carbon black composite electromagnetic wave absorbing material prepared in the embodiment, and as can be seen from fig. 1, the high-entropy alloy/carbon black composite electromagnetic wave absorbing material prepared in the embodiment has a maximum reflection loss value of-50.91 dB when the thickness of a coating is 2mm, the corresponding frequency is 5.51GHz, the effective wave absorbing frequency width is 2.36GHz, and meanwhile, 2.36GHz is also the maximum effective wave absorbing frequency width.
Example 2
The embodiment comprises the following steps:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material; the mass purity of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black is more than 99.5 percent; the particle size of the carbon black is less than 1 mu m; the premixing is to grind alternately clockwise and anticlockwise in a mortar for 30min, and the alternation of clockwise and anticlockwise is performed every 5min;
step two, adding the raw materials, ethanol and stainless steel grinding balls obtained in the step one into a ball milling tank for stirring, and then sealing the ball milling tank in a glove box filled with argon to obtain a sealed ball milling tank;
step three, mounting the sealed ball milling tank obtained in the step two on a high-energy ball mill for high-energy ball milling, opening the sealed ball milling tank after the high-energy ball milling in a glove box filled with argon, and obtaining precursor powder in the sealed ball milling tank; ball-to-material ratio in the high-energy ball milling process is 11:1, a step of; the rotating speed of the high-energy ball milling is 300r/min, the ball milling time is 90h, and the ball milling stays for 3min every 60 min;
step four, sequentially carrying out vacuum drying and screening on the precursor powder obtained in the step three to obtain high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder; the conditions of the vacuum drying are as follows: heating to 80 ℃ under the condition of vacuum degree of 1Pa, and preserving heat for 12 hours; the screening process comprises the following steps: and screening by adopting a 100-mesh filter screen, a 200-mesh filter screen and a 300-mesh filter screen in sequence, wherein the grain size of the high-entropy alloy/carbon black composite electromagnetic wave absorbing material powder is smaller than 10 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is (FeNiCrAl) 0.5 ) 95 C 5 。
The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is mixed with paraffin to prepare a test sample with the inner diameter of 3mm, the outer diameter of 7mm and the thickness of 2mm, then the wave-absorbing performance of the test sample is detected, the maximum reflection loss value of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in the embodiment is-31.76 dB, the corresponding frequency is 3.58GHz, the effective wave-absorbing frequency is 1.12GHz, and meanwhile, the 1.12GHz is the maximum effective wave-absorbing frequency, the maximum reflection loss is smaller than-10 dB required by the wave-absorbing material, so that the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment has excellent wave-absorbing performance.
Fig. 2 is a graph of wave absorbing performance of the high-entropy alloy/carbon black composite electromagnetic wave absorbing material prepared in this embodiment, and as can be seen from fig. 2, the high-entropy alloy/carbon black composite electromagnetic wave absorbing material prepared in this embodiment has a maximum reflection loss value of-31.76 dB when the coating thickness is 2mm, and corresponds to a frequency of 3.58GHz, and an effective wave absorbing frequency width of 1.12GHz, and at the same time, 1.12GHz is also the maximum effective wave absorbing frequency width.
Example 3
The embodiment comprises the following steps:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material; the mass purity of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black is more than 99.5 percent; the particle size of the carbon black is less than 1 mu m; the premixing is to grind alternately clockwise and anticlockwise in a mortar for 40min, and the alternation of clockwise and anticlockwise is performed every 5min;
step two, adding the raw materials, ethanol and stainless steel grinding balls obtained in the step one into a ball milling tank for stirring, and then sealing the ball milling tank in a glove box filled with argon to obtain a sealed ball milling tank;
step three, mounting the sealed ball milling tank obtained in the step two on a high-energy ball mill for high-energy ball milling, opening the sealed ball milling tank after the high-energy ball milling in a glove box filled with argon, and obtaining precursor powder in the sealed ball milling tank; the ball-material ratio in the high-energy ball milling process is 15:1, a step of; the rotating speed of the high-energy ball milling is 450r/min, the ball milling time is 60h, and the ball milling stays for 1min every 50 min;
step four, sequentially carrying out vacuum drying and screening on the precursor powder obtained in the step three to obtain high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder; the conditions of the vacuum drying are as follows: heating to 70 ℃ under the condition of vacuum degree of 1Pa, and preserving heat for 12 hours; the screening process comprises the following steps: and screening by adopting a 100-mesh filter screen, a 200-mesh filter screen and a 300-mesh filter screen in sequence, wherein the grain size of the high-entropy alloy/carbon black composite electromagnetic wave absorbing material powder is smaller than 5 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is (FeNiCrAl) 0.1 ) 99 C 1 。
The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is mixed with paraffin to prepare a test sample with the inner diameter of 3mm, the outer diameter of 7mm and the thickness of 2mm, and then the test sample is subjected to wave-absorbing performance detection, the maximum reflection loss value of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in the embodiment is-42.75 dB, the corresponding frequency is 2.43GHz, the effective wave-absorbing frequency is 2.98GHz, and meanwhile, the 2.98GHz is the maximum effective wave-absorbing frequency, the maximum reflection loss is smaller than-10 dB required by the wave-absorbing material, so that the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment has excellent wave-absorbing performance.
Example 4
The embodiment comprises the following steps:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material; the mass purity of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black is more than 99.5 percent; the particle size of the carbon black is less than 1 mu m; the premixing is to grind alternately clockwise and anticlockwise in a mortar for 50min, and the alternation of clockwise and anticlockwise is carried out every 5min;
step two, adding the raw materials, ethanol and stainless steel grinding balls obtained in the step one into a ball milling tank for stirring, and then sealing the ball milling tank in a glove box filled with argon to obtain a sealed ball milling tank;
step three, mounting the sealed ball milling tank obtained in the step two on a high-energy ball mill for high-energy ball milling, opening the sealed ball milling tank after the high-energy ball milling in a glove box filled with argon, and obtaining precursor powder in the sealed ball milling tank; the ball-material ratio in the high-energy ball milling process is 18:1, a step of; the rotating speed of the high-energy ball milling is 350r/min, the ball milling time is 70h, and the ball milling stays for 5min every 60 min;
step four, sequentially carrying out vacuum drying and screening on the precursor powder obtained in the step three to obtain high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder; the conditions of the vacuum drying are as follows: heating to 60 ℃ under the condition of vacuum degree of 1Pa, and preserving heat for 12 hours; the screening process comprises the following steps: and screening by adopting a 100-mesh filter screen, a 200-mesh filter screen and a 300-mesh filter screen in sequence, wherein the grain size of the high-entropy alloy/carbon black composite electromagnetic wave absorbing material powder is 5-10 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is (FeNiCrAl) 0.1 ) 95 C 5 。
The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is mixed with paraffin to prepare a test sample with the inner diameter of 3mm, the outer diameter of 7mm and the thickness of 2mm, and then the test sample is subjected to wave-absorbing performance detection, the maximum reflection loss value of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in the embodiment is-37.21 dB, the corresponding frequency is 6.35GHz, the effective wave-absorbing frequency is 1.47GHz, and meanwhile, the 1.47GHz is the maximum effective wave-absorbing frequency, the maximum reflection loss is smaller than-10 dB required by the wave-absorbing material, so that the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment has excellent wave-absorbing performance.
Example 5
The embodiment comprises the following steps:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material; the mass purity of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black is more than 99.5 percent; the particle size of the carbon black is less than 1 mu m; the premixing is to grind alternately clockwise and anticlockwise in a mortar for 60min, and the alternation of clockwise and anticlockwise is performed every 5min;
step two, adding the raw materials, ethanol and stainless steel grinding balls obtained in the step one into a ball milling tank for stirring, and then sealing the ball milling tank in a glove box filled with argon to obtain a sealed ball milling tank;
step three, mounting the sealed ball milling tank obtained in the step two on a high-energy ball mill for high-energy ball milling, opening the sealed ball milling tank after the high-energy ball milling in a glove box filled with argon, and obtaining precursor powder in the sealed ball milling tank; the ball-material ratio in the high-energy ball milling process is 16:1, a step of; the rotating speed of the high-energy ball milling is 420r/min, the ball milling time is 80h, and the ball milling stays for 1min every 60 min;
step four, sequentially carrying out vacuum drying and screening on the precursor powder obtained in the step three to obtain high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder; the conditions of the vacuum drying are as follows: heating to 60 ℃ under the condition of vacuum degree of 1Pa, and preserving heat for 12 hours; the screening process comprises the following steps: and screening by adopting a 100-mesh filter screen, a 200-mesh filter screen and a 300-mesh filter screen in sequence, wherein the grain size of the high-entropy alloy/carbon black composite electromagnetic wave absorbing material powder is smaller than 5 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is (FeNiCrAl) 0.1 ) 90 C 10 。
The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is mixed with paraffin to prepare a test sample with the inner diameter of 3mm, the outer diameter of 7mm and the thickness of 2mm, and then the test sample is subjected to wave-absorbing performance detection, the maximum reflection loss value of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in the embodiment is-47.82 dB, the corresponding frequency is 5.26GHz, the effective wave-absorbing frequency is 3.15GHz, and meanwhile, the 3.15GHz is the maximum effective wave-absorbing frequency, the maximum reflection loss is smaller than-10 dB required by the wave-absorbing material, so that the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment has excellent wave-absorbing performance.
Example 6
The embodiment comprises the following steps:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material; the mass purity of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black is more than 99.5 percent; the particle size of the carbon black is less than 1 mu m; the premixing is that clockwise and anticlockwise alternate grinding is carried out in a mortar for 35min, and the clockwise and anticlockwise alternate grinding is carried out at intervals of 5min;
step two, adding the raw materials, ethanol and stainless steel grinding balls obtained in the step one into a ball milling tank for stirring, and then sealing the ball milling tank in a glove box filled with argon to obtain a sealed ball milling tank;
step three, mounting the sealed ball milling tank obtained in the step two on a high-energy ball mill for high-energy ball milling, opening the sealed ball milling tank after the high-energy ball milling in a glove box filled with argon, and obtaining precursor powder in the sealed ball milling tank; the ball-material ratio in the high-energy ball milling process is 12:1, a step of; the rotating speed of the high-energy ball milling is 330r/min, the ball milling time is 65h, and the ball milling time is 30min each time and the ball milling time is 1min each time;
step four, sequentially carrying out vacuum drying and screening on the precursor powder obtained in the step three to obtain high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder; the conditions of the vacuum drying are as follows: heating to 70 ℃ under the condition of vacuum degree of 0.9Pa, and preserving heat for 12 hours; the screening process comprises the following steps: and screening by adopting a 100-mesh filter screen, a 200-mesh filter screen and a 300-mesh filter screen in sequence, wherein the grain size of the high-entropy alloy/carbon black composite electromagnetic wave absorbing material powder is less than 5-15 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is (FeNiCrAl) 0.3 ) 95 C 5 。
The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is mixed with paraffin to prepare a test sample with the inner diameter of 3mm, the outer diameter of 7mm and the thickness of 2mm, and then the test sample is subjected to wave-absorbing performance detection, the maximum reflection loss value of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in the embodiment is-39.49 dB, the corresponding frequency is 2.87GHz, the effective wave-absorbing frequency is 2.02GHz, and meanwhile, the 2.02GHz is the maximum effective wave-absorbing frequency, the maximum reflection loss is smaller than-10 dB required by the wave-absorbing material, so that the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment has excellent wave-absorbing performance.
Example 7
The embodiment comprises the following steps:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material; the mass purity of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black is more than 99.5 percent; the particle size of the carbon black is less than 1 mu m; the premixing is to grind alternately clockwise and anticlockwise in a mortar for 45min, and the alternation of clockwise and anticlockwise is carried out every 5min;
step two, adding the raw materials, ethanol and stainless steel grinding balls obtained in the step one into a ball milling tank for stirring, and then sealing the ball milling tank in a glove box filled with argon to obtain a sealed ball milling tank;
step three, mounting the sealed ball milling tank obtained in the step two on a high-energy ball mill for high-energy ball milling, opening the sealed ball milling tank after the high-energy ball milling in a glove box filled with argon, and obtaining precursor powder in the sealed ball milling tank; the ball-material ratio in the high-energy ball milling process is 15:1, a step of; the rotating speed of the high-energy ball milling is 380r/min, the ball milling time is 75h, and the ball milling is stopped for 4min every 50 min;
step four, sequentially carrying out vacuum drying and screening on the precursor powder obtained in the step three to obtain high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder; the conditions of the vacuum drying are as follows: heating to 60 ℃ under the condition of vacuum degree of 1Pa, and preserving heat for 12 hours; the screening process comprises the following steps: and screening by adopting a 100-mesh filter screen, a 200-mesh filter screen and a 300-mesh filter screen in sequence, wherein the grain size of the high-entropy alloy/carbon black composite electromagnetic wave absorbing material powder is smaller than 10 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is (FeNiCrAl) 0.3 ) 93 C 7 。
The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is mixed with paraffin to prepare a test sample with the inner diameter of 3mm, the outer diameter of 7mm and the thickness of 2mm, and then the test sample is subjected to wave-absorbing performance detection, the maximum reflection loss value of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in the embodiment is-35.42 dB, the corresponding frequency is 6.80GHz, the effective wave-absorbing frequency is 2.75GHz, and meanwhile, the 2.75GHz is the maximum effective wave-absorbing frequency, the maximum reflection loss is smaller than-10 dB required by the wave-absorbing material, so that the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment has excellent wave-absorbing performance.
Example 8
The embodiment comprises the following steps:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material; the mass purity of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black is more than 99.5 percent; the particle size of the carbon black is less than 1 mu m; the premixing is to grind alternately clockwise and anticlockwise in a mortar for 55min, and the alternation of clockwise and anticlockwise is carried out every 5min;
step two, adding the raw materials, ethanol and stainless steel grinding balls obtained in the step one into a ball milling tank for stirring, and then sealing the ball milling tank in a glove box filled with argon to obtain a sealed ball milling tank;
step three, mounting the sealed ball milling tank obtained in the step two on a high-energy ball mill for high-energy ball milling, opening the sealed ball milling tank after the high-energy ball milling in a glove box filled with argon, and obtaining precursor powder in the sealed ball milling tank; the ball-material ratio in the high-energy ball milling process is 20:1, a step of; the rotating speed of the high-energy ball milling is 400r/min, the ball milling time is 85h, and the ball milling time is 50min each time and the ball milling time is 5min each time;
step four, sequentially carrying out vacuum drying and screening on the precursor powder obtained in the step three to obtain high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder; the conditions of the vacuum drying are as follows: heating to 80 ℃ under the condition of vacuum degree of 0.8Pa, and preserving heat for 12 hours; the screening process comprises the following steps: and screening by adopting a 100-mesh filter screen, a 200-mesh filter screen and a 300-mesh filter screen in sequence, wherein the grain size of the high-entropy alloy/carbon black composite electromagnetic wave absorbing material powder is smaller than 5-10 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is (FeNiCrAl) 0.5 ) 90 C 10 。
The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment is mixed with paraffin to prepare a test sample with the inner diameter of 3mm, the outer diameter of 7mm and the thickness of 2mm, and then the test sample is subjected to wave-absorbing performance detection, the maximum reflection loss value of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in the embodiment is-44.31 dB, the corresponding frequency is 5.86GHz, the effective wave-absorbing frequency is 2.74GHz, and meanwhile, the 2.74GHz is the maximum effective wave-absorbing frequency, the maximum reflection loss is smaller than-10 dB required by the wave-absorbing material, so that the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared in the embodiment has excellent wave-absorbing performance.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (7)
1. The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material is characterized in that the molecular formula of the high-entropy alloy/carbon black is (FeNiCrAl a ) x C y Wherein a is the molar ratio of Al to Fe, ni and Cr, and x and y are FeNiCrAl in the high-entropy alloy/carbon black respectively a And C, the a satisfies: a is more than or equal to 0.1 and less than or equal to 0.5; the x satisfies the following conditions: x is more than or equal to 90 and less than or equal to 99, and y satisfies the following conditions: y is 1-10 and x+y=100; regulating said (FeNiCrAl) a ) x The atomic percentage of Al element and the mass percentage of carbon black in the C limit the content of Al in the quaternary high-entropy alloy, so that the Al and Ni in the quaternary high-entropy alloy fully form Ni 2 An Al phase;
the preparation method of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material comprises the following steps:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material;
step two, adding the raw materials, ethanol and stainless steel grinding balls obtained in the step one into a ball milling tank for stirring, and then sealing the ball milling tank in a glove box filled with argon to obtain a sealed ball milling tank;
step three, mounting the sealed ball milling tank obtained in the step two on a high-energy ball mill for high-energy ball milling, opening the sealed ball milling tank after the high-energy ball milling in a glove box filled with argon, and obtaining precursor powder in the sealed ball milling tank;
and step four, sequentially carrying out vacuum drying and screening on the precursor powder obtained in the step three to obtain the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder.
2. The high-entropy alloy/carbon black composite electromagnetic wave absorbing material according to claim 1, wherein the mass purity of the metallic iron, metallic nickel, metallic chromium, metallic aluminum and carbon black in the first step is more than 99.5%; the particle size of the carbon black is less than 1 mu m.
3. The high-entropy alloy/carbon black composite electromagnetic wave absorbing material according to claim 1, wherein the premixing in the first step is performed by alternately grinding clockwise and counterclockwise in a mortar for 30-60 min.
4. The high-entropy alloy/carbon black composite electromagnetic wave absorbing material according to claim 1, wherein in the step three, the ball-to-material ratio in the high-energy ball milling process is 10-20: 1.
5. the high-entropy alloy/carbon black composite electromagnetic wave absorbing material according to claim 1, wherein the rotating speed of the high-energy ball milling in the third step is 300-450 r/min, the ball milling time is 60-90 h, and each ball milling time in the high-energy ball milling is 30-60 min, and the ball milling time is stopped for 1-5 min.
6. The high-entropy alloy/carbon black composite electromagnetic wave absorbing material according to claim 1, wherein the vacuum drying conditions in the fourth step are: heating to 60-80 ℃ under the condition of 0.8-1 Pa of vacuum degree, and preserving heat for 12h.
7. The high-entropy alloy/carbon black composite electromagnetic wave absorbing material according to claim 1, wherein the screening in the fourth step is performed by: sieving with 100 mesh, 200 mesh and 300 mesh sieve.
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