CN114309586A - 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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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 121
- 239000000956 alloy Substances 0.000 title claims abstract description 121
- 239000011358 absorbing material Substances 0.000 title claims abstract description 98
- 239000002131 composite material Substances 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title abstract description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 60
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 46
- 229910052742 iron Inorganic materials 0.000 claims abstract description 33
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- 239000000463 material Substances 0.000 claims abstract description 25
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 23
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- 239000011651 chromium Substances 0.000 claims abstract description 19
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 19
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- 238000000227 grinding Methods 0.000 claims description 32
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- 230000008569 process Effects 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 25
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- 238000010438 heat treatment Methods 0.000 claims description 10
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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)xCyWherein 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 respectivelyaThe material has the advantages that the quaternary high-entropy alloy is formed by Fe, Ni, Cr and Al and is compounded with carbon black, so that the material 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 addition, the invention also provides a preparation method of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material,the method realizes the preparation of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material by carrying out high-energy ball milling on metallic iron, metallic nickel, metallic chromium, metallic aluminum and carbon black, and 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 the living space of people, causing a great amount of electromagnetic wave pollution, and the electromagnetic pollution becomes the fourth most pollution following the atmospheric pollution, water pollution and noise pollution. The 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 the pollution of electromagnetic waves in the surrounding environment, so that people are free from the harm of the electromagnetic waves, therefore, the high-efficiency wave-absorbing material also becomes a hot point of social attention, and the wave-absorbing material has very important value in both military and civil fields.
The electromagnetic absorbent plays a decisive role in the wave-absorbing material, and the electromagnetic absorbent mainly has three types: magnetic absorbers, electrically conductive absorbers, and dielectric absorbers. However, the magnetism of the magnetic absorbent disappears at high temperature, and the loss of the conductive absorbent and the dielectric absorbent is small, and the absorption capacity is poor, so that a novel wave absorbing material needs to be developed.
High-entropy alloys are the direction of research developed and rapidly raised in recent years, and show advantages over traditional alloys in mechanical, physical and chemical properties. With the deep research of the high-entropy alloy, the high-entropy alloy is no longer limited by the five-membered equiatomic ratio, and the quaternary high-entropy alloy is especially developed by the non-equiatomic ratio high-entropy alloy, so that the wave-absorbing material has larger space in component selection. The composition of the high-entropy alloy and the carbon substance, namely the composition design combining 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 formed by compounding a quaternary high-entropy alloy consisting of Fe, Ni, Cr and Al and carbon black, 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 technical scheme that: 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)xCyWherein 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 respectivelyaAnd mass fraction of C.
The invention forms a quaternary high-entropy alloy by Fe, Ni, Cr and Al, has more ideal soft magnetic performance, meets the condition of forming a magnetic medium loss type wave-absorbing material, adopts carbon black as a material of an electrical loss mechanism, and adopts FeNiCrAlaThe combination of the quaternary high-entropy alloy and the carbon black can provide multiple loss mechanisms, improve the wave-absorbing performance of the material and provide a high-entropy alloy/carbon black composite electromagnetic wave-absorbing material with excellent performance.
The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material is characterized in that a meets the following requirements: a is more than or equal to 0.1 and less than or equal to 0.5; the x satisfies: x is more than or equal to 90 and less than or equal to 99, and y satisfies the following condition: y is more than or equal to 1 and less than or equal to 10, and x + y is 100. The invention limits the content of Al in the quaternary high-entropy alloy by controlling the numerical range of a, so that Al and Ni in the quaternary high-entropy alloy can fully form Ni2The Al phase is precipitated on the matrix, the resistivity of the alloy is improved due to disordered arrangement, the hysteresis loss of the alloy is effectively reduced, the guarantee is provided for the service of the alloy in a high-temperature environment, the magnetic loss in the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material is dominant by controlling the numerical ranges of x and y, and the wave-absorbing advantage of the novel wave-absorbing material of the high-entropy alloy in severe environments such as high temperature is guaranteed to be exerted.
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 of:
premixing metal iron, metal nickel, metal chromium, metal aluminum and carbon black to obtain a raw material;
step two, adding the raw materials obtained in the step one, ethanol and stainless steel grinding balls 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, then 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 by the collision of grinding balls in the ball milling process, and the FeNiCrAl is formed by chemical over-reactionaQuaternary high-entropy alloy, carbon black and FeNiCrAlaThe invention improves the electromagnetic wave absorbing performance of the magnetic metal material by alloying and material compounding, prepares the high-entropy alloy powder by a mechanical alloying method, introduces a large amount of crystal defects into the high-entropy alloy powder, can be used as a polarization center to enhance the polarization effect, thereby improving the electromagnetic wave absorbing performance of the material, has electrical loss while the alloy has the magnetic loss by compounding the carbon black, thereby improving the electromagnetic wave absorbing performance of the material, has excellent wave absorbing performance and wide application prospect, and further expands the application field of the high-entropy alloy, provides a new method for the development of high-entropy alloyA thinking; the invention has the advantages that the ethanol is added in the ball milling process, the effect of a control agent is realized, the alloy is prevented from being oxidized in the high-energy ball milling process, and cold welding and blocking in the high-energy ball milling process can be prevented, so that the ball-milled powder is dispersed.
The method is characterized in that the mass purities of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black in the step one are all more than 99.5%; the particle size of the carbon black is less than 1 mu m. The invention controls the quality purity of the metal iron, the metal nickel, the metal chromium, the metal aluminum and the carbon black, thereby controlling the purity of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material and ensuring the performance of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material.
The method is characterized in that in the step one, the premixing is performed by alternately grinding clockwise and anticlockwise for 30-60 min in a mortar. According to the invention, by alternately grinding clockwise and anticlockwise, the grinding balls are more fully contacted with the powder, and more uniform alloying and material compounding are ensured, 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 the ratio of balls to materials in the high-energy ball milling process in the third step is 10-20: 1. the invention adopts higher ball-to-material ratio, provides larger energy in the ball milling process, ensures the smooth proceeding of alloying and realizes the preparation of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material.
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 h-90 h, and the ball milling is stopped for 1 min-5 min every 30 min-60 min in the high-energy ball milling. The invention ensures the alloying and compounding to be smoothly carried out by controlling the rotating speed, and prevents the defects that the alloying process cannot be smoothly finished due to too small rotating speed, the ball-milling tank is damaged due to too large impact force of a ball mill to generate serious scrap iron pollution and the component content of the high-entropy alloy wave-absorbing material is influenced due to too large rotating speed.
The method is characterized in that the vacuum drying conditions in the fourth step are as follows: heating to 60-80 ℃ under the condition that the vacuum degree is 0.8-1 Pa, and then preserving heat for 12 h. The invention makes full use of the ethanol in the raw materials through vacuum drying so as to facilitate the test and detection of the subsequent samples.
The method is characterized in that the screening process in the fourth step is as follows: screening by using 100-mesh, 200-mesh and 300-mesh filter screens in sequence. The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder with the required particle size is obtained by 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 by the collision of grinding balls in the ball milling process, and the FeNiCrAl is formed by chemical over-reactionaQuaternary high-entropy alloy, carbon black and FeNiCrAlaThe quaternary high-entropy alloy is compounded in a high-energy ball mill in a physical mode 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 by alloying and material compounding, prepares the high-entropy alloy powder by a mechanical alloying method, introduces a large amount of crystal defects into the high-entropy alloy powder, and the defects can be used as polarization centers to enhance the polarization effect, thereby improving the electromagnetic wave-absorbing performance of the material.
3. The invention has the advantages that the ethanol is added in the ball milling process, the effect of a control agent is realized, the alloy is prevented from being oxidized in the high-energy ball milling process, and cold welding and blocking in the high-energy ball milling process can be prevented, so that the ball-milled powder is dispersed.
4. Regulation of the inventionThe atomic percentage content of Al element and the mass percentage content of carbon black in the radar wave-absorbing coating material limit the Al content in the quaternary high-entropy alloy, so that Al and Ni in the quaternary high-entropy alloy can fully form Ni2The Al phase is precipitated on the matrix, the resistivity of the alloy is improved due to disordered arrangement, the hysteresis loss of the alloy is effectively reduced, the guarantee is provided for the service of the alloy in a high-temperature environment, the magnetic loss in the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material is dominant, and the wave-absorbing advantage of the novel wave-absorbing material of the high-entropy alloy in severe environments such as high temperature is guaranteed.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a wave-absorbing performance curve of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in example 1 of the invention.
FIG. 2 is a wave-absorbing performance curve of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in example 2 of the 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 purities of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black are all more than 99.5%; 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 60min, and the clockwise and anticlockwise alternate grinding is carried out every 5 min;
step two, adding the raw materials obtained in the step one, ethanol and stainless steel grinding balls 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, then 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-to-material ratio in the high-energy ball milling process is 10: 1; the rotation speed of the high-energy ball milling is 400r/min, the ball milling time is 60h, and the ball milling lasts 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 vacuum drying conditions are as follows: heating to 70 ℃ under the condition that the vacuum degree is 1Pa, and then preserving heat for 12 h; the screening process comprises the following steps: and screening by using 100-mesh, 200-mesh and 300-mesh filter screens in sequence, wherein the particle size of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder is less than 5 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared by the embodiment is (FeNiCrAl)0.3)99C1。
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 bandwidth is 2.36GHz, meanwhile, the 2.36GHz is also the maximum effective wave-absorbing bandwidth, and the maximum reflection loss is less than-10 dB required by the wave-absorbing material, which shows 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 this embodiment, and as can be seen from fig. 1, when the coating thickness of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in this embodiment is 2mm, the maximum reflection loss value is-50.91 dB, the corresponding frequency is 5.51GHz, the effective wave-absorbing bandwidth is 2.36GHz, and 2.36GHz is also the maximum effective wave-absorbing bandwidth.
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 purities of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black are all more than 99.5%; 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 30min, and the clockwise and anticlockwise alternate grinding is carried out every 5 min;
step two, adding the raw materials obtained in the step one, ethanol and stainless steel grinding balls 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, then 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-to-material ratio in the high-energy ball milling process is 11: 1; the rotation speed of the high-energy ball milling is 300r/min, the ball milling time is 90h, and the ball milling lasts 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 vacuum drying conditions are as follows: heating to 80 ℃ under the condition that the vacuum degree is 1Pa, and then preserving heat for 12 h; the screening process comprises the following steps: and screening by using 100-mesh, 200-mesh and 300-mesh filter screens in sequence, wherein the particle size of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder is less than 10 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared by the embodiment is (FeNiCrAl)0.5)95C5。
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-31.76 dB, the corresponding frequency is 3.58GHz, the effective wave-absorbing bandwidth is 1.12GHz, meanwhile, 1.12GHz is also the maximum effective wave-absorbing bandwidth, and the maximum reflection loss is less than-10 dB required by the wave-absorbing material, which shows 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 wave-absorbing performance curve of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in this embodiment, and it can be seen from fig. 2 that when the coating thickness of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material prepared in this embodiment is 2mm, the maximum reflection loss value is-31.76 dB, the corresponding frequency is 3.58GHz, the effective wave-absorbing bandwidth is 1.12GHz, and meanwhile, 1.12GHz is also the maximum effective wave-absorbing bandwidth.
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 purities of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black are all more than 99.5%; 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 for 40min in a mortar, and the clockwise and anticlockwise alternate grinding is carried out once every 5 min;
step two, adding the raw materials obtained in the step one, ethanol and stainless steel grinding balls 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, then 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-to-material ratio in the high-energy ball milling process is 15: 1; the rotation speed of the high-energy ball milling is 450r/min, the ball milling time is 60h, and the ball milling lasts 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 vacuum drying conditions are as follows: heating to 70 ℃ under the condition that the vacuum degree is 1Pa, and then preserving heat for 12 h; the screening process comprises the following steps: and screening by using 100-mesh, 200-mesh and 300-mesh filter screens in sequence, wherein the particle size of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder is less than 5 mu m.
Through detection, the high entropy prepared by the embodimentThe molecular formula of the alloy/carbon black composite electromagnetic wave-absorbing material powder is (FeNiCrAl)0.1)99C1。
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 bandwidth is 2.98GHz, meanwhile, the 2.98GHz is also the maximum effective wave-absorbing bandwidth, and the maximum reflection loss is less than-10 dB required by the wave-absorbing material, which shows 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 purities of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black are all more than 99.5%; 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 for 50min in a mortar, and the clockwise and anticlockwise alternate grinding is carried out once every 5 min;
step two, adding the raw materials obtained in the step one, ethanol and stainless steel grinding balls 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, then 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-to-material ratio in the high-energy ball milling process is 18: 1; the rotation speed of the high-energy ball milling is 350r/min, the ball milling time is 70h, and the ball milling lasts 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 vacuum drying conditions are as follows: heating to 60 ℃ under the condition that the vacuum degree is 1Pa, and then preserving heat for 12 h; the screening process comprises the following steps: and screening by using 100-mesh, 200-mesh and 300-mesh filter screens in sequence, wherein the particle 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 by the embodiment is (FeNiCrAl)0.1)95C5。
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 bandwidth is 1.47GHz, meanwhile, 1.47GHz is also the maximum effective wave-absorbing bandwidth, and the maximum reflection loss is less than-10 dB required by the wave-absorbing material, which shows 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 purities of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black are all more than 99.5%; 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 60min, and the clockwise and anticlockwise alternate grinding is carried out every 5 min;
step two, adding the raw materials obtained in the step one, ethanol and stainless steel grinding balls 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, then 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-to-material ratio in the high-energy ball milling process is 16: 1; the rotating speed of the high-energy ball milling is 420r/min, the ball milling time is 80h, and the ball milling lasts 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 vacuum drying conditions are as follows: heating to 60 ℃ under the condition that the vacuum degree is 1Pa, and then preserving heat for 12 h; the screening process comprises the following steps: and screening by using 100-mesh, 200-mesh and 300-mesh filter screens in sequence, wherein the particle size of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder is less than 5 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared by the embodiment is (FeNiCrAl)0.1)90C10。
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 bandwidth is 3.15GHz, meanwhile, the 3.15GHz is also the maximum effective wave-absorbing bandwidth, and the maximum reflection loss is less than-10 dB required by the wave-absorbing material, which shows 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 purities of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black are all more than 99.5%; the particle size of the carbon black is less than 1 mu m; the premixing is that 35min clockwise and anticlockwise alternate grinding is carried out in a mortar, and the clockwise and anticlockwise alternate grinding is carried out every 5 min;
step two, adding the raw materials obtained in the step one, ethanol and stainless steel grinding balls 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, then 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-to-material ratio in the high-energy ball milling process is 12: 1; the rotation speed of the high-energy ball milling is 330r/min, the ball milling time is 65h, and each ball milling time is 30min and is kept for 1 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 vacuum drying conditions are as follows: heating to 70 ℃ under the condition that the vacuum degree is 0.9Pa, and then preserving heat for 12 h; the screening process comprises the following steps: and screening by using 100-mesh, 200-mesh and 300-mesh filter screens in sequence, wherein the particle 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 by the embodiment is (FeNiCrAl)0.3)95C5。
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 bandwidth is 2.02GHz, meanwhile, the 2.02GHz is also the maximum effective wave-absorbing bandwidth, and the maximum reflection loss is less than-10 dB required by the wave-absorbing material, which shows 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 purities of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black are all more than 99.5%; 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 for 45min in a mortar, and the clockwise and anticlockwise alternate grinding is carried out once every 5 min;
step two, adding the raw materials obtained in the step one, ethanol and stainless steel grinding balls 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, then 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-to-material ratio in the high-energy ball milling process is 15: 1; the rotation speed of the high-energy ball milling is 380r/min, the ball milling time is 75h, and each ball milling time is 50min and the ball milling time is 4 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 vacuum drying conditions are as follows: heating to 60 ℃ under the condition that the vacuum degree is 1Pa, and then preserving heat for 12 h; the screening process comprises the following steps: and screening by using 100-mesh, 200-mesh and 300-mesh filter screens in sequence, wherein the particle size of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder is less than 10 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared by the embodiment is (FeNiCrAl)0.3)93C7。
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 bandwidth is 2.75GHz, meanwhile, the 2.75GHz is also the maximum effective wave-absorbing bandwidth, and the maximum reflection loss is less than-10 dB required by the wave-absorbing material, which shows 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 purities of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black are all more than 99.5%; 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 for 55min in a mortar, and the clockwise and anticlockwise alternate grinding is carried out once every 5 min;
step two, adding the raw materials obtained in the step one, ethanol and stainless steel grinding balls 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, then 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-to-material ratio in the high-energy ball milling process is 20: 1; the rotation speed of the high-energy ball milling is 400r/min, the ball milling time is 85h, and each ball milling time is 50min and 5 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 vacuum drying conditions are as follows: heating to 80 ℃ under the condition that the vacuum degree is 0.8Pa, and then preserving heat for 12 h; the screening process comprises the following steps: and screening by using 100-mesh, 200-mesh and 300-mesh filter screens in sequence, wherein the particle size of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder is less than 5-10 mu m.
Through detection, the molecular formula of the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material powder prepared by the embodiment is (FeNiCrAl)0.5)90C10。
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 bandwidth is 2.74GHz, meanwhile, 2.74GHz is also the maximum effective wave-absorbing bandwidth, and the maximum reflection loss is less than-10 dB required by the wave-absorbing material, which shows 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 for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (9)
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)xCyWherein 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 respectivelyaAnd mass fraction of C.
2. The high-entropy alloy/carbon black composite electromagnetic wave-absorbing material of claim 1, wherein a satisfies: a is more than or equal to 0.1 and less than or equal to 0.5; the x satisfies: x is more than or equal to 90 and less than or equal to 99, and y satisfies the following condition: y is more than or equal to 1 and less than or equal to 10, and x + y is 100.
3. A method for preparing the high-entropy alloy/carbon black composite electromagnetic wave-absorbing material as claimed in any one of claim 1 or claim 2, wherein the method 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 obtained in the step one, ethanol and stainless steel grinding balls 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, then 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.
4. The method of claim 3, wherein the mass purities of the metallic iron, the metallic nickel, the metallic chromium, the metallic aluminum and the carbon black in the first step are all more than 99.5%; the particle size of the carbon black is less than 1 mu m.
5. The method according to claim 3, wherein the premixing in the first step is alternately clockwise and counterclockwise grinding in a mortar for 30-60 min.
6. The method according to claim 3, wherein the ratio of balls to materials in the high-energy ball milling process in step three is 10-20: 1.
7. the method as claimed in claim 3, wherein the rotation speed of the high-energy ball milling in the third step is 300r/min to 450r/min, the ball milling time is 60h to 90h, and the ball milling is stopped for 1min to 5min every 30min to 60 min.
8. The method according to claim 3, wherein the vacuum drying conditions in step four are as follows: heating to 60-80 ℃ under the condition that the vacuum degree is 0.8-1 Pa, and then preserving heat for 12 h.
9. The method of claim 3, wherein the screening in step four comprises: screening by using 100-mesh, 200-mesh and 300-mesh filter screens in sequence.
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| CN115161531A (en) * | 2022-07-08 | 2022-10-11 | 西安稀有金属材料研究院有限公司 | High-entropy alloy/graphene composite material with wave absorption performance and preparation method thereof |
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