CN113956027A - Ferrite wave-absorbing material and preparation method thereof - Google Patents
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- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 51
- 239000011358 absorbing material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 9
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 4
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000009766 low-temperature sintering Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 238000010521 absorption reaction Methods 0.000 abstract description 6
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- 238000004519 manufacturing process Methods 0.000 abstract description 5
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- 238000001816 cooling Methods 0.000 abstract 1
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- 238000005303 weighing Methods 0.000 abstract 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000004891 communication Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 239000012071 phase Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
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- 210000000987 immune system Anatomy 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- 235000006408 oxalic acid Nutrition 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 210000004994 reproductive system Anatomy 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- 229940039790 sodium oxalate Drugs 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2683—Other ferrites containing alkaline earth metals or lead
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3213—Strontium oxides or oxide-forming salts thereof
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
The invention relates to a ferrite wave-absorbing material and a preparation method thereof. The ferrite wave-absorbing material has a chemical formula of SrxFeyO; the preparation method comprises the following steps: (1) selecting SrCO3And Fe2O3As a raw material, according to the chemical formula SrxFeyCalculating the stoichiometric ratio of Sr and Fe in O, and weighing each raw material; (2) adding the raw materials into a ball milling tank, adding absolute ethyl alcohol and zirconium balls, performing ball milling and drying, grinding by using a mortar, putting into a crucible, placing into a muffle furnace, sintering in an air atmosphere, and naturally cooling after sintering; (3) and ball-milling, grinding and refining the sintered powder to obtain the wave-absorbing ferrite powder. By using the present inventionThe wave-absorbing ferrite with excellent microwave absorption capacity and wide effective frequency bandwidth can be obtained by the formula and the preparation method, has the advantages of high stability, excellent performance, simple process and low production cost, and has higher practical value and wide application prospect in the field of electromagnetic shielding and stealth.
Description
Technical Field
The invention relates to the technical field of radar wave-absorbing materials, in particular to a ferrite wave-absorbing material and a preparation method thereof.
Background
With the development and progress of society, the electronic information and microwave communication technology is rapidly developed, electronic equipment continuously emerges in daily life, and electromagnetic waves are widely applied in the life fields of aerospace, military, medical and health fields, communication and the like. The electromagnetic interference (EMI) phenomenon caused by the electromagnetic interference becomes one of the serious problems. This affects the stability of information communication, for example, in important fields such as aerospace, and even safety accidents may occur. Research shows that the human immune system, the reproductive system and the nervous system are damaged under the condition of a large amount of electromagnetic radiation for a long time. Therefore, the electromagnetic interference not only affects the normal operation of the precise electronic instrument, but also poses a great threat to the health of people. The wave-absorbing material can convert microwaves into other energy such as heat energy and the like, so that the electromagnetic interference of electronic equipment and target detection characteristics such as radar are greatly reduced or eliminated, and therefore, the wave-absorbing material is one of important materials in the technical fields of electromagnetic protection, military stealth and civil use.
Ferrite materials are the main wave absorbers due to their better performance and lower cost. Currently, most studied among ferrites are spinel type ferrites and magnetolead type ferrites. The ferrite crystal structure and the saturation magnetization are controlled by regulating and controlling the doping ions and the doping amount thereof, and the microwave absorption performance is further improved within a certain range. For example, CN103482969A discloses a rare earth samarium element doped Co synthesized by solid phase method2The ferrite with the Z-shaped planar hexagonal structure has the maximum reflection loss of-19 dB to-21 dB within the range of 5-8 GHz. CN 112142456A discloses a modified ferrite doped with La, Ti, Cu and other elements, which reaches-22 dB to-41 dB near 10-15 GHz, but still has thicker matching thickness at a frequency of 18GHz, poor practicability and higher cost.
Currently, most ferrites are prepared by a chemical precipitation method, a hydrothermal method and a sol-gel method, for example, CN 111533177 a discloses a microwave absorbing material for generating submicron hollow cobalt ferrite by using the hydrothermal method; CN 109037961 a discloses a method for preparing an oxalate double salt precursor by a coprecipitation method using a mixed solution of oxalic acid (sodium oxalate) and a soluble metal salt, then burning organic matters such as oxalate in an oxygen atmosphere by a slow-heating roasting heat treatment process to turn into gas and discharge the gas, and obtaining a nickel-zinc ferrite with a large amount of microporous structures in the process. The preparation methods have the advantages of small production scale, low efficiency and high cost.
Disclosure of Invention
The invention aims to solve the technical problem of providing a perovskite-like ferrite wave-absorbing material aiming at the defects in the prior art. The wave-absorbing material has the maximum reflection loss of-20 dB to 40dB in the range of 12 GHz to 18 GHz.
The technical scheme adopted by the invention for solving the problems is as follows:
a ferrite wave-absorbing material has a chemical formula of SrxFeyAnd O, the ferrite is of a perovskite-like structure, wherein x and y are mole numbers, wherein x is 3.6-4.4, and y is 5.6-6.4.
The ferrite wave-absorbing material has the maximum reflection loss of-20 to-30 dB and the effective frequency bandwidth of more than 3.8GHz within the range of 13-18 GHz.
The preparation method of the ferrite wave-absorbing material comprises the following steps:
(1) according to the formula of the component SrxFeySelecting SrCO from the stoichiometric ratio of atoms in O3、Fe2O3Mixing the raw materials (namely SrCO)3、Fe2O3The molar ratio of (a) to (b) is x:0.5y), wherein x is 3.6 to 4.4, and y is 5.6 to 6.4.
(2) Raw material SrCO3、Fe2O3Ball-milling and mixing uniformly, then heating to 1050-1150 ℃ for sintering, and keeping the temperature for 2-3 hours;
(3) and (3) grinding the sintered powder obtained in the step (2) by using a mortar, performing ball milling for 12-24 hours, drying, and then grinding again to obtain the ferrite wave-absorbing powder material.
According to the scheme, in the step (1), the purity of the raw materials is not lower than 99%.
According to the scheme, in the step (1), SrCO is adjusted3、Fe2O3The fluctuation of x and y in the value range is realized.
According to the scheme, in the step (2) and the step (3), ball milling is carried out in absolute ethyl alcohol, and the mass ratio of the powder to the zirconium balls to the absolute ethyl alcohol is 2: 1: 1.5. in addition, the ratio of large to small zirconium balls is 1: 3: 1.
according to the scheme, in the step (2) and the step (3), the rotating speed of the ball milling tank is 100-120 r/min, and the ball milling time is 12-24 h.
According to the scheme, in the step (2), the heating rate is 1-3 ℃/min.
According to the scheme, the sintering in the step (2) is divided into a low-temperature sintering stage of 0-1000 ℃ and a high-temperature sintering stage of 1000-1150 ℃; the heating rate of the low-temperature sintering stage is 2-3 ℃/min, and the heating rate of the high-temperature sintering stage is 1-2 ℃/min; and the heat preservation time is 2-3 hours after the highest temperature is reached.
According to the scheme, in the step (3), the grinding time of two times is 2-3 hours, and a mortar is adopted for grinding.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the strontium ferrite with the perovskite-like structure is successfully synthesized, so that the wave absorbing performance of the material can be realized, and the strontium ferrite has stronger microwave absorbing capacity in different fields, namely within the range of 12-18 GHz. The preparation method of the invention adopts the traditional solid-phase sintering method, has simple process and high production efficiency, solves the problem of mass production, and has low energy consumption and low production cost.
Drawings
FIG. 1 is an X-ray diffraction analysis spectrum of the ferrite wave-absorbing material prepared in example 1;
FIG. 2 is a scanning electron microscope atlas of the ferrite wave-absorbing material prepared in example 1;
FIG. 3 is a vector network analysis spectrum of the ferrite wave-absorbing material prepared in example 1 at a frequency of 0.1 GHz-18 GHz;
FIG. 4 is a graph of reflection loss of the ferrite wave-absorbing material prepared in example 1 under the simulation of Matlab frequency of 0.1 GHz-18 GHz with different thicknesses;
FIG. 5 is a Cole-Cole curve of the ferrite wave-absorbing material prepared in example 1 at a frequency of 0.1GHz to 18 GHz.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the content of the present invention, but the present invention is not limited to the following examples.
In the following examples, in step (2) and step (3), ball milling was performed in absolute ethanol, and the mass ratio of the powder to the zirconium balls to the absolute ethanol was 2: 1: 1.5. in addition, the ratio of large to small zirconium balls is 1: 3: 1.
example 1
The ferrite wave-absorbing material comprises Sr4Fe6O13。
The preparation method of the ferrite wave-absorbing material comprises the following steps:
(1) according to the chemical expression of Sr4Fe6O13Selecting Sr carbonate and Fe in stoichiometric ratio2O3As a raw material;
(2) ball-milling the raw materials weighed in the step (1) for 12 hours, uniformly mixing, drying the premix in an oven at the drying temperature of 80-100 ℃, grinding the premix for 2 hours by using a mortar after drying, and then putting the premix into a muffle furnace to heat to 1100 ℃; wherein the temperature rise procedure is divided into a low-temperature sintering stage at 0-1000 ℃ and a high-temperature sintering stage at 1000-1100 ℃; the heating rate of the low-temperature sintering stage is 2-3 ℃/min, the heating rate of the high-temperature sintering stage is 1-2 ℃/min, and the temperature is kept for 2 hours after the temperature is raised to 1100 ℃;
(3) and grinding the sintered powder for 12 hours, performing secondary ball milling, drying, and grinding for 2 hours to reduce the particle size to obtain the ferrite wave-absorbing material.
The ferrite wave-absorbing material obtained in the step (3) of the embodiment 1 is subjected to phase analysis by an X-ray diffractometer, and as shown in FIG. 1, pure phase Sr can be formed at 1100 DEG C4Fe6O13Is of perovskite-like structure; the size and the shape state of the crystal grain are analyzed by a scanning electron microscope, as shown in figure 2, Sr of the ferrite wave-absorbing material4Fe6O13The crystal grain has a flaky structure and the size of the crystal grain is about 2 mu m.
In the ferrite wave-absorbing material obtained in the step (3) in the embodiment 1, the scattering parameters of transmission and reflection of the sample are measured by a coaxial line method, the electromagnetic parameters of the sample are reversely calculated, and a coaxial sample is manufactured by a tablet press for testing, wherein the coaxial sample has the coaxial inner diameter of 3.04mm, the coaxial outer diameter of 7mm and the coaxial thickness of 3mm, and as shown in fig. 3, the ferrite wave-absorbing material has the dielectric constant of 10-22 and the dielectric loss of 0.2 within the range of 0.1-18 GHz.
The ferrite wave-absorbing material obtained in the step (3) in the embodiment 1 is subjected to vector network test and Matlab simulation to obtain a reflection loss map, as shown in FIG. 4, reflection loss absorption peaks are gradually shifted to low frequency along with the increase of the thickness, the reflection loss has an absorption peak of-20 dB near 18GHz at the thickness of 0.14mm, and the reflection loss has an absorption peak of-22 dB near 13GHz at the thickness of 0.2 mm.
The ferrite wave-absorbing material obtained in the step (3) in the embodiment 1 passes through a vector network test, the obtained real part of the dielectric constant is taken as an abscissa, and the imaginary part of the dielectric constant is taken as an ordinate, and a Cole-Cole curve is drawn, as shown in FIG. 5, the drawn curve shows a Cole-Cole semicircular trend, and the radian is strong on the whole, which shows that the polarization has strong contribution to the dielectric loss and the electromagnetic absorption performance, and the sample has strong dielectric loss capability.
In addition, by adjusting SrCO3、Fe2O3The molar ratio of the materials can be adjusted to prepare the ferrite wave-absorbing material SrxFeyThe values of x and y in O can prepare the ferrite wave-absorbing material with similar performance and structure as those of the embodiment 1.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and changes can be made without departing from the inventive concept of the present invention, and these modifications and changes are within the protection scope of the present invention.
Claims (8)
1. A ferrite wave-absorbing material is characterized in that: the ferrite is perovskite-like strontium ferrite and has the chemical formula as follows: srxFeyO; wherein x and y are mole numbers, wherein x is 3.6-4.4, and y is 5.6-6.4.
2. The ferrite wave-absorbing material of claim 1, wherein: the wave-absorbing material has the maximum reflection loss of-20 to-30 dB and the effective frequency bandwidth of over 3.8GHz within the range of 13-18 GHz.
3. The preparation method of the ferrite wave-absorbing material according to claim 1, characterized by comprising the following steps:
(1) according to the formula of the component SrxFeySelecting SrCO from the stoichiometric ratio of atoms in O3、Fe2O3Mixing raw materials, wherein x is 3.6-4.4, and y is 5.6-6.4;
(2) raw material SrCO3、Fe2O3Ball-milling and mixing uniformly, then heating to 1050-1150 ℃ for sintering, and keeping the temperature for 2-3 hours;
(3) and (3) grinding the sintered powder obtained in the step (2), and grinding again after ball milling and drying to obtain the ferrite wave-absorbing material.
4. The preparation method of the ferrite wave-absorbing material according to claim 3, characterized in that: in the step (1), the purity of the raw materials is not lower than 99%.
5. The preparation method of the ferrite wave-absorbing material according to claim 3, characterized in that: in the step (2) and the step (3), absolute ethyl alcohol is used as a solvent for ball milling, and the mass ratio of the powder to the ball milling balls to the absolute ethyl alcohol is 1: (0.4-0.6): (0.7-0.8).
6. The preparation method of the ferrite wave-absorbing material according to claim 3, characterized in that: in the step (2) and the step (3), the rotating speed of the ball milling tank is 100-120 r/min, and the ball milling time is 12-24 h.
7. The preparation method of the ferrite wave-absorbing material according to claim 3, characterized in that: the sintering in the step (2) is divided into a low-temperature sintering stage at 0-1000 ℃ and a high-temperature sintering stage at more than 1000 ℃; the heating rate of the low-temperature sintering stage is 2-3 ℃/min, and the heating rate of the high-temperature sintering stage is 1-2 ℃/min; and the heat preservation time is 2-3 hours after the highest temperature is reached.
8. The preparation method of the ferrite wave-absorbing material according to claim 3, characterized in that: in the step (3), the two times of grinding are both 2-3 hours, and a mortar is adopted for grinding.
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Cited By (3)
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CN114538912A (en) * | 2022-01-07 | 2022-05-27 | 中国科学技术大学 | Layered perovskite-like structure oxide and preparation method and application thereof |
CN114735968A (en) * | 2022-03-15 | 2022-07-12 | 广州城建职业学院 | Building material with electromagnetic absorption function and waterproof function and preparation method thereof |
CN116395750A (en) * | 2023-03-27 | 2023-07-07 | 桂林电子科技大学 | SmCaFeO wave-absorbing material and preparation method thereof |
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