CN112408409B - High-temperature-resistant high-entropy wave-absorbing ceramic and preparation method and application thereof - Google Patents
High-temperature-resistant high-entropy wave-absorbing ceramic and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a high-temperature-resistant high-entropy wave-absorbing ceramic and a preparation method and application thereof, wherein the high-entropy ceramic is prepared from the following raw materials in molar ratio: 0.98-1.02 parts of cerium oxide, 0.98-1.02 parts of yttrium oxide, 0.98-1.02 parts of samarium oxide, 0.98-1.02 parts of erbium oxide, 0.98-1.02 parts of ytterbium oxide and 15 parts of boron carbide. The high-entropy ceramic has the advantages of low density, high purity, strong wave absorption performance and wide absorption frequency band, the maximum wave absorption loss is 28-34dB, and the maximum absorption frequency band width is 3.5-3.9 GHz. The invention utilizes the high-entropy technology, simultaneously introduces not less than 5 rare earth metal elements into hexaboride, obtains the high-temperature-resistant high-entropy wave-absorbing ceramic through a high-temperature electric furnace under the vacuum condition, has better high-temperature stability of reaction products due to the influence of the high-entropy effect, has lower required reaction conditions, simple process, high speed and strong practicability, is suitable for industrial production, and has good application prospect in the field of wave-absorbing materials.
Description
Technical Field
The invention belongs to the field of microwave absorbing materials and preparation and application thereof, relates to high-temperature-resistant high-entropy wave absorbing ceramic and a preparation method and application thereof, and particularly relates to high-entropy ceramic with low density, high purity, strong wave absorbing performance and wide absorption band and a preparation method and application thereof.
Background
With the development of modern science and technology, various electronic and electrical devices provide great help for people's daily life, but at the same time, the problems of electromagnetic radiation and interference generated by the devices also generate new problems for people's production and life, and the living space of human beings is worsened. In addition, in the military field, due to the need of radar stealth, the aircraft needs to avoid the action of electromagnetic waves. Therefore, the development of wave-absorbing materials is needed to absorb electromagnetic wave signals. The ideal wave-absorbing material should have the characteristics of being thin, light, wide and strong, and with the development of the technology, the wave-absorbing material of the future new generation also needs to have the characteristics of environmental adaptability, high temperature resistance, oxidation resistance and the like.
At present, wave-absorbing materials are mainly classified into the following two categories: one is a carbon material, such as graphite, carbon black, graphene and the like, as a main wave-absorbing material; the other is a ferrite magnetic material. The two materials can obtain the wave absorbing efficiency of more than-20 dB after the nanocrystallization treatment. However, both materials have their intrinsic defects when applied at high temperatures: the wave-absorbing material mainly comprising the carbon material loses the wave-absorbing capability thereof due to the oxidation of the carbon material at high temperature, and the ferrite magnetic nano material can cause the rapid attenuation of the wave-absorbing performance due to the weakening of the magnetism and the growth of nano material grains at high temperature.
The rare earth hexaboride not only has the characteristics of low density, good high-temperature stability and the like, but also has large adjustability of the size of metal atoms contained in crystal lattices, has good performance regulation and control space, is favorable for controlling the performance of the rare earth hexaboride in a large range by adding different metals, and does not have research and report on the electromagnetic absorption performance at present.
Disclosure of Invention
The invention provides a high-temperature-resistant high-entropy wave-absorbing ceramic material which has the advantages of high temperature resistance, low density, high purity, strong wave-absorbing performance, wide absorption frequency band and the like.
The invention also aims to provide a preparation method of the high-temperature-resistant high-entropy wave-absorbing ceramic, which is characterized in that no less than 5 rare earth metal elements are simultaneously introduced into hexaboride through a high-entropy technology, and the high-entropy ceramic has matched electrical property and magnetic property through selection of raw materials, so that the wave-absorbing property of the high-entropy ceramic is improved, and the high-temperature-resistant high-entropy wave-absorbing ceramic material is obtained.
The invention further aims to provide application of the high-temperature-resistant high-entropy wave-absorbing ceramic material.
In order to achieve the above purpose, the invention provides the following technical scheme:
a high-temperature-resistant high-entropy wave-absorbing ceramic is prepared from the following raw materials in molar ratio:
0.98-1.02 parts of cerium oxide;
0.98-1.02 parts of yttrium oxide;
0.98-1.02 parts of samarium oxide;
0.98-1.02 parts of erbium oxide;
0.98-1.02 parts of ytterbium oxide;
and 15 parts of boron carbide.
The types of the cations or metal ions in the high-temperature-resistant high-entropy wave-absorbing ceramic compound are more than or equal to 5.
The high-temperature-resistant high-entropy wave-absorbing ceramic compound has the use temperature of more than or equal to 1000 ℃.
In the high-temperature-resistant high-entropy wave-absorbing ceramic, cerium oxide, yttrium oxide, samarium oxide, erbium oxide, ytterbium oxide and boron carbide in raw material components are powder, the purity of the cerium oxide, the yttrium oxide, the samarium oxide, the erbium oxide and the ytterbium oxide is not lower than 99.9%, and the granularity of the cerium oxide, the yttrium oxide, the samarium oxide, the erbium oxide and the ytterbium oxide is not larger than 1 micron; the purity of the boron carbide is not less than 98 percent, and the powder can be sieved by a 120-mesh sieve.
The preparation method of the high-temperature-resistant high-entropy wave-absorbing ceramic comprises the following steps:
(1) mixing the raw material powder with absolute ethyl alcohol in a ball milling tank to obtain uniformly mixed slurry;
(2) drying and sieving the obtained slurry to obtain mixed powder, and calcining the powder in a high-temperature electric furnace to obtain ceramic powder;
in the preparation method of the high-temperature-resistant high-entropy wave-absorbing ceramic, in the step (2), the calcining temperature is 1900-2000 ℃, and the calcining time is 1-2 h.
In the preparation method of the high-temperature-resistant high-entropy wave-absorbing ceramic, in the step (2), the calcination vacuum degree is controlled to be 8-15 Pa.
The high-temperature-resistant high-entropy wave-absorbing ceramic material is used for a wave-absorbing coating.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the invention, more than 5 rare earth elements and the B element are combined to form a novel single compound, and the corresponding rare earth elements are introduced into the structure according to the required product performance to obtain the high-entropy compound with adjustable performance. First with Y2O3、Yb2O3、Sm2O3、Er2O3、Eu2O3And B4C is used as raw material, and has low density, high purity, strong wave absorption performance and wide absorptionAnalysis shows that the prepared high-temperature-resistant high-entropy wave-absorbing ceramic has the maximum wave-absorbing loss of 28-34dB and the maximum absorption frequency bandwidth of 3.5-3.9 GHz.
(2) The invention utilizes the high-entropy technology, simultaneously introduces not less than 5 rare earth metal elements into hexaboride, and obtains the high-temperature-resistant high-entropy wave-absorbing ceramic through a high-temperature electric furnace under the vacuum condition. Through the selection of raw materials, the high-entropy ceramic has matched electrical property and magnetic property, and the wave-absorbing property of the high-entropy ceramic is improved. Due to the high entropy effect, the high-temperature stability of the reaction product is better, so the required reaction condition is lower, the process is simple and quick, the practicability is strong, and the method is suitable for large-scale production and application.
Drawings
FIG. 1 is an X-ray diffraction spectrum of the high-temperature-resistant high-entropy wave-absorbing ceramic prepared in example 1 of the present invention;
FIG. 2 is a powder microstructure diagram and a particle distribution diagram of the high-temperature-resistant high-entropy wave-absorbing ceramic prepared in example 1 of the present invention;
FIG. 3 is a return loss spectrogram of the high-temperature-resistant high-entropy wave-absorbing ceramic prepared in embodiment 1 of the present invention.
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The high-temperature-resistant high-entropy wave-absorbing ceramic is prepared from the following raw materials in molar ratio:
0.98-1.02 parts of cerium oxide;
0.98-1.02 parts of yttrium oxide;
0.98-1.02 parts of samarium oxide;
0.98-1.02 parts of erbium oxide;
0.98-1.02 parts of ytterbium oxide;
and 15 parts of boron carbide.
The types of the cations or metal ions in the high-temperature-resistant high-entropy wave-absorbing ceramic compound are more than or equal to 5.
The high-temperature-resistant high-entropy wave-absorbing ceramic compound has the use temperature of more than or equal to 1000 ℃.
In the raw material components, cerium oxide, yttrium oxide, samarium oxide, erbium oxide, ytterbium oxide and boron carbide are powder, the purity of the cerium oxide, the yttrium oxide, the samarium oxide, the erbium oxide and the ytterbium oxide is not lower than 99.9%, and the granularity is not larger than 1 micron; the purity of the boron carbide is not less than 98 percent, and the powder can be sieved by a 120-mesh sieve.
The preparation method of the high-temperature-resistant high-entropy wave-absorbing ceramic comprises the following steps:
(1) mixing the raw material powder with absolute ethyl alcohol in a ball milling tank to obtain uniformly mixed slurry;
(2) drying and sieving the obtained slurry to obtain mixed powder, and calcining the powder in a high-temperature electric furnace to obtain ceramic powder;
in the step (2), the calcining temperature is 1900-2000 ℃, the calcining time is 1-2h, and the calcining vacuum degree is controlled to be 8-15 Pa. The sintering temperature and the sintering time mainly affect the purity of the ceramic material, the sintering temperature is too low and is lower than the minimum value of the range, the raw material powder cannot fully react to obtain pure high-entropy hexaboron ceramic, the sintering temperature is too short and is shorter than the minimum value of the range, the raw material powder cannot fully react to obtain pure high-entropy hexaboron ceramic, and the sintering temperature and the sintering time are too long and are higher than the maximum value of the range, so that the energy consumption level can be obviously improved, but the purity of the ceramic powder cannot be further improved.
The high-temperature-resistant high-entropy wave-absorbing ceramic material has the maximum wave-absorbing loss of 28-34dB and the maximum absorption frequency bandwidth of 3.5-3.9GHz, and has important popularization and application prospects in the field of wave-absorbing coatings.
Example 1
Will Y2O3、Sm2O3、Eu2O3、Yb2O3、Er2O3And B4C is according to Y2O3:Sm2O3:Eu2O3:Yb2O3:Er2O3:B4Weighing the mixture according to the molar ratio of C to C of 1:1:1:1:15, mixing in a ball milling tank for 6 hours, and obtaining slurry by using anhydrous ethanol as a mixing medium; filtering the obtained slurry, drying, sieving with 120 mesh sieve to obtain mixture powder, calcining the dried powder in a high temperature furnace at 1900 deg.C for 2 hr under vacuum degree of 8Pa to obtain high entropy hexaboride ceramic (Y)1/5Sm1/5Eu1/5Yb1/5Er1/5)B6The powder has the ceramic purity of 100 wt% and the average grain diameter of 1.86 microns, and the maximum wave absorption loss is 33.4dB under the frequency of 2-18GHz by using an Agilent N5244A vector network analyzer, and the maximum absorption frequency bandwidth is 3.9GHz when the reflectivity is below-10 dB. The obtained high-entropy ceramic components are shown in an X-ray diffraction spectrum of figure 1, the micro-morphology and the particle size distribution of the high-entropy ceramic are shown in figure 2, and the wave absorption loss of the high-entropy ceramic at the frequency of 2-18GHz is shown in a return loss spectrum of figure 3. The high-temperature resistant high-entropy wave-absorbing ceramic with the purity not less than 99 wt% can be prepared when the high-temperature reaction temperature is 1900 ℃.
Example 2
Will Y2O3、Sm2O3、Eu2O3、Yb2O3、Er2O3And B4C is according to Y2O3:Sm2O3:Eu2O3:Yb2O3:Er2O3:B4Weighing the mixture according to the molar ratio of C to 1:1:1:1:15, mixing in a ball milling tank for 6 hours, and obtaining slurry by using anhydrous pure ethanol as a mixing medium; filtering the obtained slurry, drying, sieving with 120 mesh sieve to obtain mixture powder, calcining the dried powder in a high temperature furnace at 2000 deg.C for 1 hr under vacuum degree of 15Pa to obtain high entropy hexaboride ceramic (Y)1/5Sm1/5Eu1/5Yb1/5Er1/5)B6The powder has the ceramic purity of 100 wt% and the average grain diameter of 2.1 microns, and has the maximum wave absorption loss of 30dB under the frequency of 2-18GHz and the maximum absorption frequency bandwidth of 3.6GHz when the reflectivity is below-10 dB, which are measured by an Agilent N5244A vector network analyzer.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.
Claims (9)
1. The high-temperature-resistant high-entropy wave-absorbing ceramic is characterized by being prepared from the following raw materials in molar ratio:
the maximum wave absorbing loss of the high-temperature-resistant high-entropy wave absorbing ceramic is 28-34dB, and the maximum absorbing frequency bandwidth is 3.5-3.9 GHz.
2. The high-temperature-resistant high-entropy wave-absorbing ceramic according to claim 1, wherein cerium oxide, yttrium oxide, samarium oxide, erbium oxide, ytterbium oxide and boron carbide in the raw material components are powder.
3. The high-temperature-resistant high-entropy wave-absorbing ceramic according to claim 1, wherein the purity of cerium oxide, yttrium oxide, samarium oxide, erbium oxide and ytterbium oxide is not less than 99.9%, and the granularity is not more than 1 micron; the purity of the boron carbide is not less than 98 percent, and the powder can be sieved by a 120-mesh sieve.
4. The preparation method of the high-temperature-resistant high-entropy wave-absorbing ceramic according to any one of claims 1 to 3, comprising the following steps:
(1) mixing the raw material powder with absolute ethyl alcohol in a ball milling tank to obtain uniformly mixed slurry;
(2) drying and sieving the obtained slurry to obtain mixed powder, and calcining the powder to obtain ceramic powder;
5. the preparation method of the high-temperature-resistant high-entropy wave-absorbing ceramic according to claim 4, wherein in the step (1), the mixing time is 6-12 h.
6. The preparation method of the high-temperature-resistant high-entropy wave-absorbing ceramic according to claim 4, wherein a filtering step is added after the step (1) is completed, and then the step (2) is carried out.
7. The preparation method of the high-temperature-resistant high-entropy wave-absorbing ceramic according to claim 4, wherein in the step (2), the calcining temperature is 1900-2000 ℃, and the calcining time is 1-2 h.
8. The preparation method of the high-temperature-resistant high-entropy wave-absorbing ceramic according to claim 4, wherein in the step (2), the calcination vacuum degree is controlled to be 8-15 Pa.
9. Use of a high temperature resistant high entropy wave absorbing ceramic material according to any one of claims 1 to 3 in a wave absorbing coating.
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| CN113754443B (en) * | 2021-08-23 | 2022-06-14 | 华南理工大学 | High-entropy hexaboride nanocrystalline ceramic and preparation method and application thereof |
| CN114736010B (en) * | 2022-04-02 | 2023-05-23 | 郑州航空工业管理学院 | High-entropy oxide ceramic, preparation method thereof and application of high-entropy oxide ceramic as electromagnetic wave absorbing material |
| CN114786454B (en) * | 2022-04-12 | 2022-10-25 | 中星(广州)纳米材料有限公司 | High-entropy alloy sulfide/two-dimensional nanocomposite and preparation method and application thereof |
| CN116655384B (en) * | 2023-06-07 | 2023-12-12 | 徐州工程学院 | High Wen Gaoshang-resistant wave-absorbing ceramic and preparation method and application thereof |
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