CN112047387A - Flower-shaped nanocrystalline Fe3S4Preparation method of wave-absorbing material - Google Patents
Flower-shaped nanocrystalline Fe3S4Preparation method of wave-absorbing material Download PDFInfo
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- CN112047387A CN112047387A CN202010812620.0A CN202010812620A CN112047387A CN 112047387 A CN112047387 A CN 112047387A CN 202010812620 A CN202010812620 A CN 202010812620A CN 112047387 A CN112047387 A CN 112047387A
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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/12—Sulfides
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
Abstract
The invention discloses flower-shaped nanocrystalline Fe3S4The preparation method of the wave-absorbing material comprises the following specific steps: first, FeCl is added3·6H2O and S (NH)2)2Dissolving in distilled water, stirring to obtain brown yellow transparent solution, adding ascorbic acid under continuous stirring until brown yellow solution is converted into colorless transparent solution, and stirring for 30 min; then transferring the colorless transparent solution into a stainless steel high-pressure kettle for hydrothermal reaction, centrifuging the suspension after the reaction, washing and drying to obtain flower-shaped nanocrystalline Fe3S4And (3) a wave-absorbing material. The invention successfully prepares the nanocrystalline Fe with a special flower-shaped structure3S4The material has good magnetism and dielectric property, realizes the principle of impedance matching, and enables electromagnetic waves to enter the material to the maximum extent when the electromagnetic waves enter the surface of the material; meanwhile, the flower-shaped structure enables the electromagnetic waves to be reflected for multiple times in the material, and the electromagnetic waves are further attenuated and lost.
Description
Technical Field
The invention belongs to the technical field of wave-absorbing material preparation, and particularly relates to flower-shaped nanoCrystalline Fe3S4A method for preparing a wave-absorbing material.
Background
At present, electronic communication technology is rapidly developing, and people are in an environment full of electromagnetic waves, and the harm of the electromagnetic waves to people is larger and larger. In life, the electromagnetic waves emitted by various electronic devices seriously affect various aspects of people, such as vision, hearing, and the like; in work, the probability of canceration of human cells is increased by electromagnetic radiation caused by various large instruments; in military, electromagnetic signals transmitted by a fighter are likely to be detected by a radar, thereby revealing the position of the fighter. However, in order to make progress in these areas, the support of the wave-absorbing material is required. Therefore, an efficient absorbing material must be found to absorb the unwanted electromagnetic signals. The wave-absorbing material is required to have high absorption rate to electromagnetic waves in a wide frequency band, and also required to have the properties of light weight, temperature resistance, moisture resistance, corrosion resistance and the like. The new generation wave-absorbing material has small thickness, light weight, strong absorption, wide frequency band and multi-spectrum development.
The wave-absorbing material needs to satisfy two principles: the impedance matching principle and the attenuation characteristic principle enable electromagnetic waves to enter the material to the maximum extent when the electromagnetic waves enter the surface of the material; the latter requires rapid and effective attenuation of electromagnetic waves entering the material. For many years, researchers have made extensive research on the electromagnetic wave absorption properties of transition metal sulfides, such as MoS2Two-dimensional nanosheet, porous Co9S8Nanotube, flower-shaped CuS hollow microsphere, hollow MnS sphere, composite material containing CuS/ZnS, and CoS2a/rGO nano hybrid material, Ni/ZnS and the like. Fe3S4The magnetic material is an important transition metal sulfide and semimetal magnetic material, and has been widely researched in the fields of high-energy batteries, electrochemical storage, sewage treatment, magnetic fluids, cracking and biomedicine due to the abundant sources, low cost, environmental friendliness and special physical and chemical properties. Fe in contrast to other transition metal sulfides3S4Has better electron conductivity, probably due to electron hopping of high spin iron and ferrous iron in an octahedral lattice. In addition, withNon-magnetic FeS and FeS2In contrast, Fe3S4Oxide (Fe) corresponding thereto3O4) And similarly have good magnetic properties. All of these indicate Fe3S4Can be used as a good wave-absorbing material to attenuate electromagnetic waves.
Disclosure of Invention
The invention aims to provide flower-shaped nanocrystalline Fe3S4The flower-shaped structure of the preparation method of the wave-absorbing material enables electromagnetic waves to be reflected for multiple times in the material, so that the electromagnetic waves are further attenuated and lost, and the wave-absorbing performance of the material is improved.
The invention adopts the technical scheme that flower-shaped nanocrystalline Fe3S4The preparation method of the wave-absorbing material is implemented according to the following steps:
step 1, FeCl3·6H2O and S (NH)2)2Dissolving in distilled water, stirring for ten minutes until the solution becomes brown yellow transparent solution, adding ascorbic acid into the brown yellow transparent solution under the state of continuous stirring until the brown yellow solution is changed into colorless transparent solution, and continuing stirring for 30 min;
The present invention is also characterized in that,
in step 1, FeCl3·6H2O、S(NH2)2And ascorbic acid in a molar ratio of 1: 5-20: 1 to 3.
In the step 2, when washing is carried out by using distilled water and ethanol, the washing frequency is not less than three times each time.
In the step 2, the reaction temperature is 160-210 ℃, and the reaction time is 3-9 h.
In step 2, the drying temperature was 60 ℃.
The beneficial effect of the invention is that,
the invention successfully prepares the nanocrystalline Fe with a special flower-shaped structure3S4The material has good magnetism and dielectric property, so that on one hand, the principle of impedance matching is realized, and electromagnetic waves can enter the material to the greatest extent when being incident to the surface of the material; on the other hand, good magnetic and dielectric properties ensure that electromagnetic waves entering the material need to be attenuated quickly and efficiently. Meanwhile, the flower-shaped structure enables the electromagnetic waves to be reflected for multiple times in the material, and the electromagnetic waves are further attenuated and lost. The method has the advantages of simple requirement on equipment, stable process, continuous operation, high production efficiency, high automation degree, cost reduction, good material uniformity and simple preparation method.
Drawings
FIG. 1 shows flower-like nanocrystalline Fe in example 1 of the present invention3S4A microscopic topography of the material (one);
FIG. 2 shows flower-like nanocrystalline Fe in example 1 of the present invention3S4A micro-topography of the material;
FIG. 3 shows flower-like nanocrystalline Fe in example 2 of the present invention3S4A magnetization profile of the material;
FIG. 4 shows flower-like nanocrystalline Fe in example 2 of the present invention3S4A wave-absorbing performance diagram of the material;
FIG. 5 shows flower-like nanocrystalline Fe in example 3 of the present invention3S4A microscopic topography of the material;
FIG. 6 shows flower-like nanocrystals of Fe in example 3 of the present invention3S4A magnetization profile of the material;
FIG. 7 shows flower-like nanocrystalline Fe in example 3 of the present invention3S4A wave-absorbing performance diagram of the material;
FIG. 8 shows flower-like nanocrystalline Fe in example 4 of the present invention3S4A microscopic topography of the material;
FIG. 9 shows flower-like nanocrystalline Fe in example 5 of the present invention3S4A microscopic topography of the material.
Detailed Description
The present invention will be described in detail with reference to the following detailed description and accompanying drawings.
The invention relates to flower-shaped nanocrystalline Fe3S4The preparation method of the wave-absorbing material is implemented according to the following steps:
step 1, iron chloride hexahydrate (FeCl)3·6H2O) and thiourea (S (NH)2)2) Dissolving in distilled water, magnetically stirring for ten minutes until the solution becomes a brown yellow transparent solution, adding ascorbic acid into the brown yellow transparent solution under the state of continuous stirring until the brown yellow solution is converted into a colorless transparent solution, and continuously stirring for 30 min;
ferric chloride hexahydrate (FeCl)3·6H2O), thiourea (S (NH)2)2) And ascorbic acid in a molar ratio of 1: 5-20: 1-3;
the reaction temperature is 160-210 ℃, and the reaction time is 3-9 h; the drying temperature is 60 ℃;
example 1
The invention relates to flower-shaped nanocrystalline Fe3S4The preparation method of the wave-absorbing material comprises the following steps:
step 1, 0.81g of ferric chloride hexahydrate (FeCl)3·6H2O) and 3.00g of thiourea (S (NH)2)2) Dissolving in 70mL of distilled water, magnetically stirring for ten minutes until the solution becomes a brown yellow transparent solution, adding 0.80g of ascorbic acid into the brown yellow transparent solution under the state of continuous stirring until the brown yellow solution is converted into a colorless transparent solution, and continuously stirring for 30 min;
Example 2
The invention relates to flower-shaped nanocrystalline Fe3S4The preparation method of the wave-absorbing material comprises the following steps:
step 1, 0.81g of ferric chloride hexahydrate (FeCl)3·6H2O) and 3.00g of thiourea (S (NH)2)2) Dissolving in 70mL of distilled water, magnetically stirring for ten minutes until the solution becomes a brown yellow transparent solution, adding 0.80g of ascorbic acid into the brown yellow transparent solution under the state of continuous stirring until the brown yellow solution is converted into a colorless transparent solution, and continuously stirring for 30 min;
when flower-shaped nanocrystalline Fe3S4When the material is kept at the temperature of 160 ℃ for 6h, the saturation magnetization is 12.5emu g as shown in figure 3-1(ii) a As shown in fig. 4, Fe at this time3S4The composite material has the best wave-absorbing performance, and the maximum absorption frequency bandwidth can reach-51 dB and-10 dB or less and is 6 GHz.
Example 3
The invention relates to flower-shaped nanocrystalline Fe3S4The preparation method of the wave-absorbing material comprises the following steps:
step 1, 0.81g of ferric chloride hexahydrate (FeCl)3·6H2O) and 3.00g of thiourea (S (NH)2)2) Dissolving in 70mL of distilled water, magnetically stirring for ten minutes until the solution becomes a brown yellow transparent solution, adding 0.80g of ascorbic acid into the brown yellow transparent solution under the state of continuous stirring until the brown yellow solution is converted into a colorless transparent solution, and continuously stirring for 30 min;
Example 4
The invention relates to flower-shaped nanocrystalline Fe3S4The preparation method of the wave-absorbing material comprises the following steps:
step 1, 0.81g of ferric chloride hexahydrate (FeCl)3·6H2O) and 3.00g of thiourea (S (NH)2)2) Dissolving in 70mL of distilled water, magnetically stirring for ten minutes until the solution becomes a brown yellow transparent solution, and stirring continuously until the solution turns brown to yellowAdding 0.80g of ascorbic acid into the transparent solution until the brown yellow solution is converted into a colorless transparent solution, and continuing stirring for 30 min;
Example 5
The invention relates to flower-shaped nanocrystalline Fe3S4The preparation method of the wave-absorbing material comprises the following steps:
step 1, 0.81g of ferric chloride hexahydrate (FeCl)3·6H2O) and 3.00g of thiourea (S (NH)2)2) Dissolving in 70mL of distilled water, magnetically stirring for ten minutes until the solution becomes a brown yellow transparent solution, adding 0.80g of ascorbic acid into the brown yellow transparent solution under the state of continuous stirring until the brown yellow solution is converted into a colorless transparent solution, and continuously stirring for 30 min;
Claims (5)
1. Flower-shaped nanocrystalline Fe3S4The preparation method of the wave-absorbing material is characterized by comprising the following steps:
step 1, FeCl3·6H2O and S (NH)2)2Dissolving in distilled water, stirring for ten minutes until the solution becomes brown yellow transparent solution, adding ascorbic acid into the brown yellow transparent solution under the state of continuous stirring until the brown yellow solution is changed into colorless transparent solution, and continuing stirring for 30 min;
step 2, transferring the colorless transparent solution obtained in the step 1 into a polytetrafluoroethylene-lined stainless steel autoclave for hydrothermal reaction, naturally cooling to room temperature after the reaction is finished, centrifuging the suspension obtained after the reaction to obtain a black brown product, washing with distilled water and ethanol respectively, and finally drying in a drying oven to obtain flower-shaped nanocrystalline Fe3S4And (3) a wave-absorbing material.
2. Flower-like nanocrystalline Fe according to claim 13S4The preparation method of the wave-absorbing material is characterized in that in the step 1, FeCl is adopted3·6H2O、S(NH2)2And ascorbic acid in a molar ratio of 1: 5-20: 1 to 3.
3. Flower-like nanocrystalline Fe according to claim 13S4The preparation method of the wave-absorbing material is characterized in that in the step 2, when washing is carried out by using distilled water and ethanol, the washing frequency is not less than three times each time.
4. Flower-like nanocrystalline Fe according to claim 13S4The preparation method of the wave-absorbing material is characterized in that in the step 2, the reaction temperature is 160-210 ℃, and the reaction time is 3-9 h.
5. Flower-like nanocrystalline Fe according to claim 13S4The preparation method of the wave-absorbing material is characterized in that in the step 2, the drying temperature is 60 ℃.
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Cited By (1)
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CN114094301A (en) * | 2021-10-28 | 2022-02-25 | 西安理工大学 | Preparation method of magnetic-dielectric composite material dielectric resonator and miniaturized antenna |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109621924A (en) * | 2018-12-28 | 2019-04-16 | 温州医科大学 | A kind of Fe3S4Magnetic effervescent tablet and its method for detecting polybrominated diphenyl ethers |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN109621924A (en) * | 2018-12-28 | 2019-04-16 | 温州医科大学 | A kind of Fe3S4Magnetic effervescent tablet and its method for detecting polybrominated diphenyl ethers |
Non-Patent Citations (3)
Title |
---|
FENG CAO, ET AL.: "3D Fe3S4 flower-like microspheres: high-yield synthesis via a biomolecule-assisted solution approach, their electrical, magnetic and electrochemical hydrogenstorage properties" * |
JIALIANG LUO,ET AL.: "Synthesis of 3D flower-like Fe3S4 microspheres and quasi-sphere Fe3S4-RGO hybrid-architectures with enhanced electromagnetic wave absorption" * |
SHANYE YANG, ET AL.: "Synergistic removal and reduction of U(VI) and Cr(VI) by Fe3S4" * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114094301A (en) * | 2021-10-28 | 2022-02-25 | 西安理工大学 | Preparation method of magnetic-dielectric composite material dielectric resonator and miniaturized antenna |
CN114094301B (en) * | 2021-10-28 | 2023-03-24 | 西安理工大学 | Preparation method of magnetic-dielectric composite material dielectric resonator and miniaturized antenna |
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