CN113862545B - High-entropy alloy wave-absorbing material with reflection loss reaching-60.9 dB and preparation method thereof - Google Patents
High-entropy alloy wave-absorbing material with reflection loss reaching-60.9 dB and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-entropy alloy wave-absorbing material with reflection loss reaching-60.9 dB, and the molecular formula of the high-entropy alloy wave-absorbing material is FeaNibCrcAldWherein a, b, c and d respectively represent the atomic percentage values of the corresponding metal elements; the invention also discloses a preparation method of the wave-absorbing material, which comprises the following steps: firstly, weighing raw material powder according to a target product; secondly, filling powder into a glove box filled with argon gas and sealing; thirdly, ball milling; and fourthly, taking out the material and opening the material in a glove box filled with argon to obtain the high-entropy alloy wave-absorbing material. The high-entropy alloy wave-absorbing material disclosed by the invention exerts the coupling effect of multiple loss mechanisms through the composition characteristics of multiple elements, synergistically improves the wave-absorbing performance of the high-entropy alloy wave-absorbing material, has a large effective absorption bandwidth and low energy consumption, and reduces the cost of raw materials; the preparation method has simple process operation, no need of complex equipment and low cost, and is beneficial to large-scale production.
Description
Technical Field
The invention belongs to the technical field of wave-absorbing materials, and particularly relates to a high-entropy alloy wave-absorbing material with reflection loss of-60.9 dB and a preparation method thereof.
Background
With the rapid development of modern electronic industry technology, the use of a large number of electronic and electrical equipment brings convenience to the life of people, and meanwhile, the electromagnetic pollution is more and more serious. In addition, the continuous progress of radar detection technology makes military combat equipment extremely vulnerable to detection, tracking, and attack by enemies. Particularly, when the wave absorbing material is applied to stealth airplanes, aircraft carriers and the like, under the large environment of high temperature and easy corrosion, a novel wave absorbing material with high temperature oxidation resistance and high corrosion resistance is urgently needed.
Research shows that due to the effect of 'entropy' in the high-entropy alloy, a series of performances of corrosion resistance, high-temperature oxidation resistance, high-temperature stability, soft magnetic performance and the like of the alloy break through the performance limit of the traditional alloy. At present, the research on the high-entropy alloy wave-absorbing material is less, and the reported FeNiCo high-entropy alloy shows better wave-absorbing performance, but still has the following problems: (1) the effective absorption band width is narrow; the maximum reflection loss value is generally not more than-60 dB, and the thickness exceeds 2 mm; (2) the energy consumption is high; the excellent wave absorbing capacity is usually shown only by carrying out subsequent heat treatment or magnetic field annealing, and the preparation process is complicated; (3) the cost is high; the Co element contained is high in price, and the subsequent treatment improves the preparation period and further improves the production cost.
Therefore, it is necessary to develop a new low-cost high-reflection loss high-entropy alloy.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a high-entropy alloy wave-absorbing material with reflection loss of-60.9 dB aiming at the defects of the prior art. The high-entropy alloy wave-absorbing material exerts the coupling effect of multiple loss mechanisms through the composition characteristics of multiple elements, the wave-absorbing performance of the high-entropy alloy wave-absorbing material is obviously and synergistically improved, the effective absorption bandwidth is large, the energy consumption is low, Co is not required to be added, the raw material cost is greatly reduced, and the use requirements of the wave-absorbing material on thinness, lightness, width and strength are met.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the high-entropy alloy wave-absorbing material with the reflection loss reaching-60.9 dB is characterized in that the molecular formula of the high-entropy alloy wave-absorbing material is FeaNibCrcAldWherein a, b, c and d respectively represent the atomic percentage values of the corresponding metal elements, and the error is within the range of +/-0.2 percentA is more than or equal to 30 and less than or equal to 40, b is more than or equal to 30 and less than or equal to 40, c is more than or equal to 25 and less than or equal to 35, d is more than or equal to 5 and less than or equal to 10, and a + b + c + d = 100; the maximum reflection loss value of a coating with the thickness of 2mm prepared by the high-entropy alloy wave-absorbing material and paraffin wax mixture reaches-60.9 dB, and the effective wave-absorbing bandwidth which is less than-10 dB reaches 4.97 GHz.
According to the high-entropy alloy wave-absorbing material, the ferromagnetic elements Fe and Ni are added, so that the high-entropy alloy wave-absorbing material is promoted to absorb electromagnetic waves, the high-entropy alloy wave-absorbing material has better electromagnetic wave absorption capacity, the corrosion resistance and the oxidation resistance of the high-entropy alloy wave-absorbing material are improved by adding the corrosion-resistant and oxidation-resistant elements Cr and Al, the application range of the high-entropy alloy wave-absorbing material is expanded, the composition characteristics of multiple elements in the high-entropy alloy wave-absorbing material play a coupling role of multiple loss mechanisms, the development requirements of alloying and compounding of the wave-absorbing material are met, the wave-absorbing performance of the high-entropy alloy wave-absorbing material is obviously and synergistically improved, the effective absorption bandwidth is larger, the energy consumption is lower, Co does not need to be added, and the raw material cost is greatly reduced.
The high-entropy alloy wave-absorbing material with the reflection loss of-60.9 dB is characterized in that a =35, b =30, c =30 and d = 5.
The high-entropy alloy wave-absorbing material with the reflection loss reaching-60.9 dB is characterized in that a microstructure of the high-entropy alloy wave-absorbing material is mainly prepared from a solid solution. The micro phase structure characteristic ensures that the wave-absorbing material belongs to the category of high-entropy alloy, thereby being beneficial to exerting the coupling effect of various loss mechanisms.
In addition, the invention also discloses a method for preparing the high-entropy alloy wave-absorbing material with the reflection loss reaching-60.9 dB, which is characterized by comprising the following steps:
converting designed atomic percentages in a target product into mass ratios, and weighing Fe, Ni, Cr and Al powder according to the mass ratios;
secondly, putting the powder of Fe, Ni, Cr and Al weighed in the step one into a ball milling tank filled with grinding balls in a glove box filled with argon, and then sealing the ball milling tank;
step three, taking the ball milling tank sealed in the step two out of the vacuum glove box, and then placing the ball milling tank on a planetary ball mill for ball milling;
and step four, cooling the ball milling tank subjected to ball milling in the step three to room temperature, then taking out the ball milling tank, placing the ball milling tank in a glove box filled with argon, opening the glove box, and taking out the powder subjected to ball milling to obtain the high-entropy alloy wave-absorbing material.
The invention directly utilizes the planetary ball mill, adopts the ball milling method to prepare the high-entropy alloy wave-absorbing material, introduces a large amount of crystal defects into the ball-milled powder by a mechanical alloying method, and the defects are used as polarization centers to enhance the polarization effect, thereby improving the electromagnetic wave-absorbing performance of the high-entropy alloy wave-absorbing material, meeting the requirements of the application field on thinness, lightness, width and strength of the wave-absorbing material, and widening the application field of the high-entropy alloy wave-absorbing material.
The method is characterized in that the mass purity of the Fe, Ni, Cr and Al powder in the step one is more than 99.5 percent. The quality and purity of the raw material powder are limited, so that the adverse effects of uncertain factors such as impurities on the performance of the wave absorbing material are reduced.
The method is characterized in that the ratio of the mass of the grinding ball to the total mass of the Fe, Ni, Cr and Al powder in the step two is 10: 1-20: 1. by controlling the mass ratio of the grinding balls to the raw material powder, a larger ball-material ratio is ensured, the raw material powder is promoted to be fully alloyed, and the quality of the high-entropy alloy wave-absorbing material is improved.
The method is characterized in that the grinding balls in the step two contain grinding balls with the diameter of 10mm, and the mass ratio of the grinding balls is 40% -60%. The mass ratio of large-size grinding balls in the grinding balls is limited, so that the mechanical impact force of the grinding balls on each raw material powder is increased, and sufficient energy is provided for the alloying process.
The method is characterized in that absolute ethyl alcohol is added into the ball milling tank before sealing in the second step to serve as a process control agent. The ball milling heat is effectively reduced by adding the absolute ethyl alcohol, the oxidation of ball milling powder is avoided, and the performance of the high-entropy alloy wave-absorbing material is ensured.
The method is characterized in that the rotating speed of the ball mill in the third step is 300 r/min-400 r/min, and the time is 10 h-90 h. The invention ensures the mechanical alloying action of the grinding balls on the raw material powder by limiting the rotation speed of the ball mill, and avoids serious scrap iron pollution caused by the damage of a ball mill tank due to overlarge impact force of the grinding balls and the influence on the component content of the high-entropy alloy wave-absorbing material; by limiting the ball milling time, the energy consumption is effectively saved, and the process flow is shortened.
The method is characterized in that in the ball milling process in the step three, the interval is 3min to 5min every 30min to 60 min. By adopting the intermittent ball milling process, the heat is effectively dissipated in the ball milling process, and the high-entropy alloy wave-absorbing material is prevented from being oxidized due to overlong ball milling time and overheating in a ball milling tank.
Compared with the prior art, the invention has the following advantages:
1. the high-entropy alloy wave-absorbing material disclosed by the invention plays a coupling effect of multiple loss mechanisms through the composition characteristics of multiple elements, particularly utilizes the 'cocktail effect' and the 'high-entropy effect' of the high-entropy alloy to synergistically increase the electromagnetic loss of the wave-absorbing material, utilizes the 'lattice distortion effect' to enhance the polarization effect, improves the electric loss capability, remarkably synergistically improves the wave-absorbing performance of the high-entropy alloy wave-absorbing material, has larger effective absorption bandwidth and lower energy consumption, does not need to add Co, and greatly reduces the cost of raw materials.
2. The maximum reflection loss value of a coating with the thickness of 2mm prepared by the high-entropy alloy wave-absorbing material and paraffin mixture reaches-60.9 dB, the effective wave-absorbing bandwidth less than-10 dB reaches 4.97GHz, the effective wave-absorbing bandwidth is improved, and the wave-absorbing material has excellent wave-absorbing performance.
3. The invention adopts a ball-milling mechanical alloying method to introduce a large amount of crystal defects into ball-milled powder, and the defects are used as polarization centers to enhance the polarization effect, thereby improving the electromagnetic wave-absorbing performance of the high-entropy alloy wave-absorbing material and meeting the application requirements of the application field on the wave-absorbing material.
4. The invention adopts ball milling to prepare the high-entropy alloy absorbing material, has the advantages of low energy consumption in the preparation process, low cost, simple operation, no need of complex equipment and low cost, and is beneficial to large-scale production.
5. The high-entropy alloy wave-absorbing material disclosed by the invention is thin in thickness, light in weight, wide in wave-absorbing frequency band and strong in wave-absorbing efficiency, meets the use requirements of the wave-absorbing material on thinness, lightness, width and strength, and meanwhile, the characteristics of multiple principal elements of the high-entropy alloy meet the alloying trend of the wave-absorbing material development.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 shows Fe prepared in example 1 of the present invention35Ni30Cr30Al5Reflection loss diagram of high entropy alloy wave-absorbing material.
FIG. 2 shows Fe prepared in examples 1 to 5 of the present invention35Ni30Cr30Al5XRD pattern of the high-entropy alloy wave-absorbing material.
FIG. 3 shows Fe prepared in examples 1 to 5 of the present invention35Ni30Cr30Al5Magnetization curve diagram of high entropy alloy wave-absorbing material.
FIG. 4 shows Fe prepared in examples 1 to 5 of the present invention35Ni30Cr30Al5And (3) a trend graph of the saturation magnetization and the coercive force of the high-entropy alloy wave-absorbing material along with the change of the ball milling time.
Detailed Description
Example 1
The molecular formula of the high-entropy alloy wave-absorbing material is Fe35Ni30Cr30Al5。
The preparation method of the high-entropy alloy wave-absorbing material comprises the following steps:
step one, a target product Fe35Ni30Cr30Al5Converting the designed atomic percentages into mass ratios, and weighing Fe, Ni, Cr and Al powder according to the mass ratios; the mass purity of the Fe, Ni, Cr and Al powder is more than 99.5 percent;
step two, under a glove box filled with argon, 30g of the powder of Fe, Ni, Cr and Al weighed in the step one is put into a ball milling tank filled with 600g of grinding balls, absolute ethyl alcohol is added as a process control agent, and then the ball milling tank is sealed; the grinding balls contain 300g of grinding balls with the diameter of 10 mm;
step three, taking the ball milling tank sealed in the step two out of the vacuum glove box, then placing the ball milling tank on a planetary ball mill, and carrying out ball milling for 90 hours at the rotating speed of 300 r/min; the ball milling process is interrupted for 5min every 60 min;
and step four, cooling the ball milling tank subjected to ball milling in the step three to room temperature, then taking out the ball milling tank, placing the ball milling tank in a glove box filled with argon, opening the glove box, and taking out the powder subjected to ball milling to obtain the flaky powder high-entropy alloy wave-absorbing material with the diameter of 3 microns.
Through detection, the saturation magnetization M of the flaky powder high-entropy alloy wave-absorbing material with the diameter of 3 mu M prepared in the embodiment is 76.01emu/g, and the coercive force H is 85.34 Oe.
FIG. 1 shows Fe prepared in example 1 of the present invention35Ni30Cr30Al5A reflection loss chart of a high-entropy alloy wave-absorbing material is shown in figure 1, the thickness of a coating prepared by the flaky powder high-entropy alloy wave-absorbing material and a paraffin mixture is different (1.5 mm-4 mm), the corresponding maximum reflection loss value, frequency and effective wave-absorbing bandwidth are different, when the thickness of the coating is 2mm, the maximum reflection loss value (RL value) is-60.9 dB, the corresponding frequency is 11.03GHz, the effective wave-absorbing bandwidth is 4.98 GHz, and the effective wave-absorbing bandwidth smaller than-10 dB is also 4.97GHz, compared with the existing high-entropy alloy wave-absorbing material, the Fe-based high-entropy alloy wave-absorbing material is characterized in that the Fe-based high-entropy alloy wave-absorbing material is prepared by using the flaky powder high-entropy alloy wave-absorbing material and the paraffin mixture, and the Fe-based high-entropy alloy wave-absorbing material has the characteristics of different thicknesses35Ni30Cr30Al5The maximum reflection loss value of the high-entropy alloy wave-absorbing material is larger, the effective wave-absorbing bandwidth range is wider, and the electromagnetic wave-absorbing performance is more excellent.
Example 2
The present embodiment is different from embodiment 1 in that: the ball milling time was 70 h.
Example 3
The present embodiment is different from embodiment 1 in that: the ball milling time is 50 h.
Example 4
The present embodiment is different from embodiment 1 in that: the ball milling time is 30 h.
Example 5
The present embodiment is different from embodiment 1 in that: the ball milling time is 10 h.
FIG. 2 shows Fe prepared in examples 1 to 5 of the present invention35Ni30Cr30Al5XRD (X-ray diffraction) pattern of high-entropy alloy wave-absorbing material, as can be seen from figure 2, Fe prepared in embodiments 1-535Ni30Cr30Al5The microstructure of the high-entropy alloy wave-absorbing material mainly adopts solid solution.
FIG. 3 shows Fe prepared in examples 1 to 5 of the present invention35Ni30Cr30Al5Magnetization curve diagram of high-entropy alloy wave-absorbing material, as can be seen from fig. 3, Fe prepared in examples 1 to 535Ni30Cr30Al5The high-entropy alloy wave-absorbing material has high saturation magnetization and low coercive force, and shows soft magnetic property.
FIG. 4 shows Fe prepared in examples 1 to 5 of the present invention35Ni30Cr30Al5A trend graph of saturation magnetization and coercive force of the high-entropy alloy wave-absorbing material along with ball milling time can be seen from FIG. 4, and Fe prepared in examples 1 to 535Ni30Cr30Al5The saturation magnetization M range of the high-entropy alloy wave-absorbing material is 69.1-94.6 emu/g, the coercive force H range is 20.9-85.4 Oe, and Fe is added along with the increase of the ball milling time35Ni30Cr30Al5The increase of impurities in the high-entropy alloy wave-absorbing material leads to the increase of internal stress, thereby leading to the increase of saturation magnetization.
Example 6
The molecular formula of the high-entropy alloy wave-absorbing material is Fe31.25Ni31.25Cr31.25Al6.25。
The preparation method of the high-entropy alloy wave-absorbing material comprises the following steps:
step one, a target product Fe31.25Ni31.25Cr31.25Al6.25Converting the designed atomic percentages into mass ratios, and weighing Fe, Ni, Cr and Al powder according to the mass ratios; the mass purity of the Fe, Ni, Cr and Al powder is more than 99.5 percent;
step two, under a glove box filled with argon, 60g of the powder of Fe, Ni, Cr and Al weighed in the step one is put into a ball milling tank filled with 600g of grinding balls, absolute ethyl alcohol is added as a process control agent, and then the ball milling tank is sealed; the grinding balls contain 360g of grinding balls with the diameter of 10 mm;
step three, taking the ball milling tank sealed in the step two out of the vacuum glove box, then placing the ball milling tank on a planetary ball mill, and carrying out ball milling for 70 hours at the rotating speed of 300 r/min; the interval is 3min every 45min during the ball milling process;
and step four, cooling the ball milling tank subjected to ball milling in the step three to room temperature, then taking out the ball milling tank, placing the ball milling tank in a glove box filled with argon, opening the glove box, and taking out the powder subjected to ball milling to obtain the flaky powder high-entropy alloy wave-absorbing material with the diameter within 10 mu m.
Through detection, the saturation magnetization M of the flaky powder high-entropy alloy wave-absorbing material with the diameter within 10 mu M prepared by the embodiment is 76.01emu/g, and the coercive force H is 85.34 Oe; the maximum reflection loss value of a coating with the thickness of 4mm prepared by the flaky powder high-entropy alloy wave-absorbing material and paraffin mixture reaches-11.5 dB, and the effective wave-absorbing bandwidth which is less than-10 dB reaches 1.82 GHz.
Example 7
The molecular formula of the high-entropy alloy wave-absorbing material is Fe30Ni30Cr30Al10。
The preparation method of the high-entropy alloy wave-absorbing material comprises the following steps:
step one, a target product Fe30Ni30Cr30Al10Converting the designed atomic percentages into mass ratios, and weighing Fe, Ni, Cr and Al powder according to the mass ratios; the mass purity of the Fe, Ni, Cr and Al powder is more than 99.5 percent;
step two, under a glove box filled with argon, 40g of powder of Fe, Ni, Cr and Al weighed in the step one is put into a ball milling tank filled with 600g of grinding balls, absolute ethyl alcohol is added as a process control agent, and then the ball milling tank is sealed; the grinding balls contain 360g of grinding balls with the diameter of 10 mm;
taking the ball milling tank sealed in the step two out of the vacuum glove box, then placing the ball milling tank on a planetary ball mill, and carrying out ball milling for 50 hours at the rotating speed of 400 r/min; the interval of 30min of each work in the ball milling process is 4 min;
and step four, cooling the ball milling tank subjected to ball milling in the step three to room temperature, then taking out the ball milling tank, placing the ball milling tank in a glove box filled with argon, opening the glove box, and taking out the powder subjected to ball milling to obtain the flaky powder high-entropy alloy wave-absorbing material with the diameter of 5 microns.
Through detection, the saturation magnetization M of the flaky powder high-entropy alloy wave-absorbing material with the diameter of 5 mu M prepared in the embodiment is 69.13emu/g, and the coercive force H is 85.36 Oe; the maximum reflection loss value of a coating with the thickness of 2.5mm prepared by the flaky powder high-entropy alloy wave-absorbing material and paraffin mixture is-12.2 dB, and the effective wave-absorbing bandwidth of less than-10 dB reaches 2.68 GHz.
Example 8
The molecular formula of the high-entropy alloy wave-absorbing material is Fe35Ni32Cr25Al8。
The preparation method of the high-entropy alloy wave-absorbing material comprises the following steps:
step one, a target product Fe35Ni32Cr25Al8Converting the designed atomic percentages into mass ratios, and weighing Fe, Ni, Cr and Al powder according to the mass ratios; the mass purity of the Fe, Ni, Cr and Al powder is more than 99.5 percent;
step two, under a glove box filled with argon, 40g of powder of Fe, Ni, Cr and Al weighed in the step one is put into a ball milling tank filled with 600g of grinding balls, absolute ethyl alcohol is added as a process control agent, and then the ball milling tank is sealed; the grinding balls contain 240g of grinding balls with the diameter of 10 mm;
taking the ball milling tank sealed in the step two out of the vacuum glove box, then placing the ball milling tank on a planetary ball mill, and carrying out ball milling for 50 hours at the rotating speed of 400 r/min; the interval is 3min every 45min during the ball milling process;
and step four, cooling the ball milling tank subjected to ball milling in the step three to room temperature, then taking out the ball milling tank, placing the ball milling tank in a glove box filled with argon, opening the glove box, and taking out the powder subjected to ball milling to obtain the flaky powder high-entropy alloy wave-absorbing material with the diameter within 8 microns.
Through detection, the saturation magnetization M of the flaky powder high-entropy alloy wave-absorbing material with the diameter within 8 mu M prepared by the embodiment is 74.89emu/g, and the coercive force H is 79.53 Oe; the maximum reflection loss value of a coating with the thickness of 4mm prepared by the flaky powder high-entropy alloy wave-absorbing material and paraffin mixture is-10.7 dB, and the effective wave-absorbing bandwidth which is less than-10 dB reaches 1.16 GHz.
Example 9
The molecular formula of the high-entropy alloy wave-absorbing material is Fe40Ni30Cr25Al5。
The preparation method of the high-entropy alloy wave-absorbing material comprises the following steps:
step one, a target product Fe40Ni30Cr25Al5Converting the designed atomic percentages into mass ratios, and weighing Fe, Ni, Cr and Al powder according to the mass ratios; the mass purity of the Fe, Ni, Cr and Al powder is more than 99.5 percent;
step two, under a glove box filled with argon, 30g of the powder of Fe, Ni, Cr and Al weighed in the step one is put into a ball milling tank filled with 600g of grinding balls, absolute ethyl alcohol is added as a process control agent, and then the ball milling tank is sealed; the grinding balls contain 300g of grinding balls with the diameter of 10 mm;
step three, taking the ball milling tank sealed in the step two out of the vacuum glove box, then placing the ball milling tank on a planetary ball mill, and carrying out ball milling for 60 hours at the rotating speed of 350 r/min; the interval is 3min every 45min during the ball milling process;
and step four, cooling the ball milling tank subjected to ball milling in the step three to room temperature, then taking out the ball milling tank, placing the ball milling tank in a glove box filled with argon, opening the glove box, and taking out the powder subjected to ball milling to obtain the flaky powder high-entropy alloy wave-absorbing material with the diameter within 5 microns.
Through detection, the saturation magnetization M of the flaky powder high-entropy alloy wave-absorbing material with the diameter within 5 mu M prepared in the embodiment is 75.12emu/g, and the coercive force H is 77.45 Oe; the maximum reflection loss value of a coating with the thickness of 2.2mm prepared by the flaky powder high-entropy alloy wave-absorbing material and paraffin mixture is-11.0 dB, and the effective wave-absorbing bandwidth of less than-10 dB reaches 1.05 GHz.
Example 10
The molecular formula of the high-entropy alloy wave-absorbing material is Fe30Ni30Cr35Al5。
The preparation method of the high-entropy alloy wave-absorbing material comprises the following steps:
step one, a target product Fe30Ni30Cr35Al5Converting the designed atomic percentages into mass ratios, and weighing Fe, Ni, Cr and Al powder according to the mass ratios; the mass purity of the Fe, Ni, Cr and Al powder is more than 99.5 percent;
step two, under a glove box filled with argon, 50g of the powder of Fe, Ni, Cr and Al weighed in the step one is put into a ball milling tank filled with 600g of grinding balls, absolute ethyl alcohol is added as a process control agent, and then the ball milling tank is sealed; the grinding balls contain 240g of grinding balls with the diameter of 10 mm;
step three, taking the ball milling tank sealed in the step two out of the vacuum glove box, then placing the ball milling tank on a planetary ball mill, and carrying out ball milling for 80 hours at the rotating speed of 400 r/min; the ball milling process is interrupted for 4min every 60 min;
and step four, cooling the ball milling tank subjected to ball milling in the step three to room temperature, then taking out the ball milling tank, placing the ball milling tank in a glove box filled with argon, opening the glove box, and taking out the powder subjected to ball milling to obtain the flaky powder high-entropy alloy wave-absorbing material with the diameter within 8 microns.
Through detection, the saturation magnetization M of the flaky powder high-entropy alloy wave-absorbing material with the diameter within 8 mu M prepared in the embodiment is 65.35emu/g, and the coercive force H is 128.64 Oe; the maximum reflection loss value of a coating with the thickness of 4mm prepared by the flaky powder high-entropy alloy wave-absorbing material and paraffin mixture is-9.8 dB, and the effective wave-absorbing bandwidth is 0GHz and is less than-10 dB.
Example 11
The molecular formula of the high-entropy alloy wave-absorbing material is Fe30Ni40Cr25Al5。
The preparation method of the high-entropy alloy wave-absorbing material comprises the following steps:
step one, a target product Fe30Ni40Cr25Al5Converting the designed atomic percentages into mass ratios, and weighing Fe, Ni, Cr and Al powder according to the mass ratios; the mass purity of the Fe, Ni, Cr and Al powder is more than 99.5 percent;
step two, under a glove box filled with argon, 30g of the powder of Fe, Ni, Cr and Al weighed in the step one is put into a ball milling tank filled with 600g of grinding balls, absolute ethyl alcohol is added as a process control agent, and then the ball milling tank is sealed; the grinding balls contain 240g of grinding balls with the diameter of 10 mm;
taking the ball milling tank sealed in the step two out of the vacuum glove box, then placing the ball milling tank on a planetary ball mill, and carrying out ball milling for 50 hours at the rotating speed of 300 r/min; the interval is 3min every 50min during the ball milling process;
and step four, cooling the ball milling tank subjected to ball milling in the step three to room temperature, then taking out the ball milling tank, placing the ball milling tank in a glove box filled with argon, opening the glove box, and taking out the powder subjected to ball milling to obtain the flaky powder high-entropy alloy wave-absorbing material with the diameter within 10 mu m.
Through detection, the saturation magnetization M of the flaky powder high-entropy alloy wave-absorbing material with the diameter within 10 mu M prepared by the embodiment is 73.22emu/g, and the coercive force H is 78.54 Oe; the maximum reflection loss value of a coating with the thickness of 2.5mm prepared by the flaky powder high-entropy alloy wave-absorbing material and paraffin mixture is-41.3 dB, and the effective wave-absorbing bandwidth is less than-10 dB and is 2.81 GHz.
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 (10)
1. The high-entropy alloy wave-absorbing material with the reflection loss reaching-60.9 dB is characterized in that the molecular formula of the high-entropy alloy wave-absorbing material is FeaNibCrcAldWherein a, b, c and d respectively represent the atomic percentage numerical values of the corresponding metal elements, the error is within the range of +/-0.2%, and a is more than or equal to 30 and less than or equal to 40, b is more than or equal to 30 and less than or equal to 40, c is more than or equal to 25 and less than or equal to 35, d is more than or equal to 5 and less than or equal to 10, and a + b + c + d = 100; the maximum reflection loss value of a coating with the thickness of 2mm prepared by the high-entropy alloy wave-absorbing material and paraffin wax mixture reaches-60.9 dB, and the effective wave-absorbing bandwidth which is less than-10 dB reaches 4.97 GHz.
2. A high entropy alloy wave absorbing material with reflection loss up to-60.9 dB according to claim 1, wherein a =35, b =30, c =30 and d = 5.
3. The high-entropy alloy wave-absorbing material with reflection loss up to-60.9 dB according to claim 1, wherein a microstructure of the high-entropy alloy wave-absorbing material is mainly solid solution.
4. A method for preparing a high entropy alloy wave absorbing material with reflection loss up to-60.9 dB according to any one of claims 1 to 3, comprising the steps of:
converting designed atomic percentages in a target product into mass ratios, and weighing Fe, Ni, Cr and Al powder according to the mass ratios;
secondly, putting the powder of Fe, Ni, Cr and Al weighed in the step one into a ball milling tank filled with grinding balls in a glove box filled with argon, and then sealing the ball milling tank;
step three, taking the ball milling tank sealed in the step two out of the vacuum glove box, and then placing the ball milling tank on a planetary ball mill for ball milling;
and step four, cooling the ball milling tank subjected to ball milling in the step three to room temperature, then taking out the ball milling tank, placing the ball milling tank in a glove box filled with argon, opening the glove box, and taking out the powder subjected to ball milling to obtain the high-entropy alloy wave-absorbing material.
5. The method according to claim 4, wherein the mass purity of the Fe, Ni, Cr and Al powders in the first step is more than 99.5%.
6. The method according to claim 4, wherein the ratio of the mass of the grinding balls to the total mass of the powders of Fe, Ni, Cr and Al in the second step is 10: 1-20: 1.
7. the method according to claim 4, wherein the grinding balls in the second step comprise grinding balls with a diameter of 10mm, and the mass ratio of the grinding balls is 40% -60%.
8. The method of claim 4, wherein absolute ethanol is added to the ball milling jar as a process control agent prior to the sealing in step two.
9. The method according to claim 4, wherein the rotation speed of the ball mill in the third step is 300r/min to 400r/min, and the time is 10h to 90 h.
10. The method according to claim 4, wherein the ball milling process in the third step is interrupted for 3min to 5min every 30min to 60 min.
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| CN115161532B (en) * | 2022-07-08 | 2023-05-12 | 西安稀有金属材料研究院有限公司 | High-entropy alloy wave-absorbing material with effective wave-absorbing frequency bandwidth and preparation method thereof |
| CN115627405B (en) * | 2022-10-21 | 2024-02-27 | 中国科学院金属研究所 | Liquid lead bismuth corrosion-resistant high-entropy alloy and preparation method thereof |
| CN116426785B (en) * | 2023-06-12 | 2023-09-08 | 西安热工研究院有限公司 | Oxygen-controlled aluminum-rich high-entropy alloy composite material and preparation method thereof |
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