CN114845538A - Magnetic metal @ carbon composite wave-absorbing material derived from layered double-magnetic metal hydroxide and preparation method thereof - Google Patents
Magnetic metal @ carbon composite wave-absorbing material derived from layered double-magnetic metal hydroxide and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a magnetic metal @ carbon composite wave-absorbing material derived from layered double magnetic metal hydroxides and a preparation method thereof.
Description
Technical Field
The invention relates to the technical field of electromagnetic wave absorbing materials, in particular to a magnetic metal @ carbon composite wave absorbing material derived from layered double-magnetic metal hydroxide and a preparation method thereof.
Background
Along with the development of radio technology and information industry, electronic products are widely applied, a series of electromagnetic radiation problems are brought along with the development of radio technology and information industry, a plurality of influences are brought to the production and the life of people, and along with the development of the electronic technology to miniaturization, integration and high frequency, the problems are more and more prominent, so that the elimination of electromagnetic interference, the avoidance of electromagnetic information leakage and the reduction of electromagnetic radiation pollution become key problems which are urgently needed to be solved in the current society.
The layered double magnetic metal hydroxide (LDH) is used as a novel material with high specific surface area and rich inner layer interfaces, can be combined with a vigorously developed material technology, and can be designed and prepared into various light high-efficiency wave-absorbing materials according to needs. LDH has the following three advantages as a wave-absorbing material: firstly, the preparation method is simple and economic, and does not need a complex experimental process; secondly, the microstructure is controllable. Nano sheets, nano wires, ultrathin structures and hollow structures are easy to form; thirdly, the components are diverse. However, in LDH precursors, only the organic ligand and the metal cation are bound, and the complex is not magnetic. The LDH derivative with unique electromagnetic performance can be obtained by modification methods such as structural design and composite materialization. Particularly, a carbon source is introduced while LDH is synthesized, and the magnetic metal carbon composite material which keeps the microscopic morphology characteristics of the precursor can be obtained through proper heat treatment, has both magnetic loss and dielectric loss, and is an ideal wave-absorbing material.
Disclosure of Invention
The invention aims to provide a layered double-magnetic metal hydroxide derived magnetic metal @ carbon composite wave-absorbing material and a preparation method thereof, namely, the layered double-magnetic metal hydroxide (LDH) is used as a precursor to synthesize the magnetic metal carbon composite wave-absorbing material with a multi-dimensional, multi-level and porous structure, so that the density of the wave-absorbing material is reduced, the multiple reflection and absorption of electromagnetic waves are realized, and the wave-absorbing performance is improved. The preparation method is simple in preparation process and low in cost, large-scale industrial production can be realized, and the prepared wave-absorbing material is small in density, thin in thickness, wide in effective absorption frequency band and strong in reflection loss.
The technical scheme for realizing the purpose of the invention is as follows:
a preparation method of a magnetic metal @ carbon composite wave-absorbing material derived from layered double-magnetic metal hydroxide comprises the following steps:
1) preparation of layered diamagnetic metal hydroxide:
sequentially adding a magnetic metal source, urea and glucose into deionized water, uniformly mixing, transferring the obtained mixed solution into a reaction kettle, carrying out hydrothermal reaction at the temperature of 160-200 ℃ for 6-24h, cooling to room temperature, carrying out suction filtration on a reaction product to obtain a dark brown precipitate, washing the dark brown precipitate with the deionized water and absolute ethyl alcohol, and drying to obtain a layered double-magnetic metal hydroxide precursor; wherein the quantity ratio of the magnetic metal source to the substances of urea and glucose is (2-6): (6-10): (1-4);
2) the preparation of the magnetic metal @ carbon composite wave-absorbing material comprises the following steps:
placing the layered double-magnetic metal hydroxide precursor prepared in the step 1) into a tubular furnace, introducing protective atmosphere Ar, heating the tubular furnace to 500-900 ℃ at the speed of 1-10 ℃/min, and calcining for 1-4h to prepare the magnetic metal @ carbon composite wave-absorbing material derived from the layered double-magnetic metal hydroxide.
In the step 1), the magnetic metal source is any two of a divalent nickel ion compound, a trivalent iron ion compound and a divalent cobalt ion compound.
The divalent nickel ion compound is any one of nickel nitrate, nickel chloride and nickel sulfate.
The ferric ion compound is any one of ferric nitrate, ferric chloride and ferric sulfate.
The divalent cobalt ion compound is any one of cobalt nitrate, cobalt chloride and cobalt sulfate.
In the step 1), the washing is carried out for 3 to 6 times.
In the step 1), the drying is carried out at the drying temperature of 60-90 ℃ for 12-24 h.
Compared with the prior art, the magnetic metal @ carbon composite wave-absorbing material derived from the layered double-magnetic metal hydroxide and the preparation method thereof have the following advantages:
1. compared with the prior art for preparing the composite wave-absorbing material, the magnetic metal carbon composite wave-absorbing material with the three-dimensional flower-shaped structure is synthesized by taking the double-magnetic metal hydroxide as the precursor, has small density, large specific surface area, rich cavity structure, various structures and various component changes, can realize the balance of dielectric loss and magnetic loss by regulating and controlling the proportion of the magnetic metal source and the carbon source, obtains good impedance matching characteristic, and has wide effective wave-absorbing frequency band and strong reflection loss.
2. The magnetic metal carbon composite wave-absorbing material prepared by the invention has a special three-dimensional flower-ball-shaped structure, and the three-dimensional flower-ball-shaped structure and the rich hole structure not only can reduce the weight and the density, but also can realize multiple reflection and absorption of incident electromagnetic waves. The carbon material wraps the magnetic alloy nano particles to form a rich heterogeneous interface, so that the interface polarization is greatly improved, and the dielectric loss is enhanced.
3. The magnetic metal carbon composite wave-absorbing material prepared by the invention has excellent wave-absorbing performance, combines an electromagnetic wave multiple reflection absorption mechanism and an interface polarization effect caused by a special three-dimensional multistage structure, natural resonance and exchange resonance generated by a magnetic alloy and electric conduction loss and dielectric loss generated by a carbon material, wherein the widest effective wave-absorbing frequency band of the FeNi @ C composite wave-absorbing material is 4.6GHz, and the strongest reflection loss is-35.4 dB.
Drawings
Fig. 1 is an XRD pattern of FeNi hydroxide precursor in example 1;
FIG. 2 is an XRD pattern of the FeNi @ C composite wave-absorbing material in the embodiment 1;
FIG. 3 is a Raman diagram of the FeNi @ C composite wave-absorbing material in the embodiment 1;
FIG. 4 is an SEM image of the FeNi @ C composite wave-absorbing material in the embodiment 1;
FIG. 5 is a reflection loss chart of the FeNi @ C composite wave-absorbing material in the embodiment 1;
FIG. 6 is an SEM image of the FeNi @ C composite wave-absorbing material in embodiment 2;
FIG. 7 is a reflection loss chart of the FeNi @ C composite wave-absorbing material in the embodiment 2;
FIG. 8 is an SEM photograph of FeCo hydroxide in example 3;
FIG. 9 is an SEM photograph of NiCo hydroxide in example 4.
Detailed Description
The invention will be further elucidated with reference to the drawings and examples, without however being limited thereto.
Example 1:
a preparation method of a magnetic metal @ carbon composite wave-absorbing material derived from layered double-magnetic metal hydroxide comprises the following steps:
1) 0.6058g of Fe (NO) are taken 3 ) 3 ·9H 2 O、0.8724g Ni (NO 3 ) 2 ·6H 2 O、0.4830g CH 4 N 2 O and 0.54g C 6 H 12 O 6 Sequentially dissolving the materials in 50ml of deionized water, magnetically stirring the materials for 30min, uniformly mixing the materials, transferring the mixed solution to a 100ml high-pressure reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 12h, carrying out vacuum filtration on a reaction product to obtain a dark brown precipitate, washing the dark brown precipitate with deionized water for three times, washing the precipitate with absolute ethyl alcohol for two times, and drying the precipitate in an oven at 60 ℃ for 12h to obtain a FeNi hydroxide (FeNi-LDH) precursor;
2) placing the FeNi-LDH precursor prepared in the step 1) in a tubular furnace, introducing protective atmosphere Ar, and sintering at 700 ℃ for 2h to finally obtain the three-dimensional flower-ball-shaped FeNi @ C composite wave-absorbing material.
Example 2:
a preparation method of a magnetic metal @ carbon composite wave-absorbing material derived from layered double-magnetic metal hydroxide comprises the following steps:
1) 0.6058g of Fe (NO) are taken 3 ) 3 ·9H 2 O、0.8724g Ni (NO 3 ) 2 ·6H 2 O、0.4830g CH 4 N 2 O and 0.54g C 6 H 12 O 6 Dissolving in 50ml deionized water in sequence, magnetically stirring for 30min, mixing, transferring the mixed solution to 100ml high-pressure reaction kettle, performing hydrothermal reaction at 180 deg.C for 12 hr, vacuum filtering the reaction product to obtain dark brown precipitate, and precipitatingWashing the precipitate with deionized water for three times, washing with absolute ethyl alcohol twice, and drying the precipitate in an oven at 60 ℃ for 12 hours to obtain a FeNi hydroxide (FeNi-LDH) precursor;
2) placing the FeNi-LDH precursor prepared in the step 1) in a tubular furnace, introducing protective atmosphere Ar, and sintering at 800 ℃ for 2h to finally obtain the three-dimensional flower-ball-shaped FeNi @ C composite wave-absorbing material.
Example 3:
a preparation method of a magnetic metal @ carbon composite wave-absorbing material derived from layered double-magnetic metal hydroxide comprises the following steps:
1) 0.6058g of Fe (NO) are taken 3 ) 3 ·9H 2 O、0.8730g Co (NO 3 ) 2 ·6H 2 O、0.4830g CH 4 N 2 O and 0.54g C 6 H 12 O 6 Sequentially dissolving the materials in 50ml of deionized water, magnetically stirring for 30min, uniformly mixing, transferring the mixed solution to a 100ml high-pressure reaction kettle, carrying out hydrothermal reaction at 180 ℃ for 12h, carrying out vacuum filtration on the reaction product to obtain a dark brown precipitate, washing the dark brown precipitate with deionized water for three times, washing the dark brown precipitate with absolute ethyl alcohol for two times, and drying the precipitate in an oven at 60 ℃ for 12h to obtain a FeCo hydroxide (FeCo-LDH) precursor;
2) placing the FeCo-LDH precursor prepared in the step 1) in a tube furnace, introducing protective atmosphere Ar, sintering at 700 ℃ and preserving heat for 2h to finally obtain the three-dimensional flower-ball-shaped FeNi @ C composite wave-absorbing material.
Example 4:
a preparation method of a magnetic metal @ carbon composite wave-absorbing material derived from layered double-magnetic metal hydroxide comprises the following steps:
1) 0.8724g of Ni (NO) were taken 3 ) 2 ·6H 2 O、0.4365g Co (NO 3 ) 2 ·6H 2 O、0.4830g CH 4 N 2 O and 0.54g C 6 H 12 O 6 Dissolving in 50ml deionized water in sequence, magnetically stirring for 30min, mixing, transferring the mixed solution to a 100ml high-pressure reaction kettle, performing hydrothermal reaction at 180 deg.C for 12 hr, vacuum filtering the reaction product to obtain dark brown precipitate,washing the dark brown precipitate with deionized water for three times, washing with absolute ethyl alcohol for two times, and drying the precipitate in a drying oven at 60 ℃ for 12h to obtain a NiCo hydroxide (NiCo-LDH) precursor;
2) putting the NiCo-LDH precursor prepared in the step 1) into a tube furnace, and introducing H 2 And sintering the/Ar mixed gas at 700 ℃ for 2h to finally obtain the three-dimensional flower spherical NiCo @ C composite wave-absorbing material.
XRD testing was performed on the FeNi-LDH precursor prepared in example 1, and the results are shown in fig. 1, where 2 θ =11.5 °, 23.2 °, 34.5 °, 39.0 ° and 60.2 °, respectively correspond to the (003), (006), (012), (015) and (110) crystal planes of nickel iron hydroxide (icdd.00-051-0463), indicating successful synthesis of the FeNi-LDH precursor.
XRD (X-ray diffraction) test is carried out on the FeNi @ C composite wave-absorbing material prepared in example 1, and the test result is shown in figure 2, wherein 2 theta = 44.2 degrees, 51.5 degrees and 75.8 degrees correspond to the FeNi respectively 3 The (111), (200) and (220) crystal planes (ICDD. 01-088-1715) of (I) indicate the presence of a successful synthesis of the FeNi alloy.
Raman tests are carried out on the FeNi @ C composite wave-absorbing material prepared in example 1, and the test results are shown in figure 3, and are 1350 cm and 1575 cm -1 The D peak and the G peak of the carbon material correspond to each other, and the result shows that glucose is converted into carbon after pyrolysis at high temperature.
SEM test is carried out on the FeNi @ C composite wave-absorbing material prepared in the embodiment 1, and the test result is shown in figure 4, and the FeNi @ C composite wave-absorbing material is of a three-dimensional flower-ball-shaped structure. The special structure can not only reduce the mass density of the wave absorbing agent, but also prolong the attenuation path of the electromagnetic wave.
The FeNi @ C composite wave-absorbing material prepared in example 1 was subjected to wave-absorbing performance test, and the reflection loss of the absorbent at 1-5mm is shown in FIG. 5. The FeNi @ C composite wave-absorbing material can reach a reflection loss of-30.4 dB at an extremely thin thickness of 1.2 mm, and has an effective wave-absorbing bandwidth of 4.6GHz at a thickness of 1.4 mm. The excellent wave-absorbing performance is related to the structure and the components. Firstly, the special three-dimensional flower-ball-shaped structure can reduce the density of the wave absorbing agent and prolong the attenuation path of the electromagnetic wave. Secondly, magnetic loss mainly based on natural resonance and exchange resonance brought by FeNi magnetic metal and dielectric loss and electric conduction loss introduced by carbon material, and finally, carbon wraps magnetic nano particles to form a large number of heterogeneous interfaces, so that an interface polarization effect is generated, and the dielectric loss capability of the wave absorbing agent is enhanced.
SEM test is carried out on the FeNi @ C composite wave-absorbing material prepared in the embodiment 2, and the test result is shown in figure 6.
The FeNi @ C composite wave-absorbing material prepared in example 2 was subjected to wave-absorbing performance test, and the test results are shown in FIG. 7. The maximum reflection loss value is only 15.7 dB, and the widest effective wave-absorbing bandwidth is 4.0 GHz. The decrease of the wave-absorbing performance is related to the structural collapse and the increase of the conductivity.
SEM tests were performed on the FeCo-LDH precursor prepared in example 3, and the test results are shown in fig. 8. The FeCo-LDH precursor is of a three-dimensional flower ball structure.
SEM tests were performed on the NiCo-LDH precursor prepared in example 4, and the test results are shown in FIG. 9. The precursor of NiCo-LDH is a three-dimensional flower ball structure.
Claims (10)
1. A preparation method of a magnetic metal @ carbon composite wave-absorbing material derived from layered double-magnetic metal hydroxide is characterized by comprising the following steps:
1) preparation of layered double hydroxide:
sequentially adding a magnetic metal source, urea and glucose into deionized water, uniformly mixing, transferring the obtained mixed solution into a reaction kettle, carrying out hydrothermal reaction at the temperature of 160-200 ℃ for 6-24h, cooling to room temperature, carrying out suction filtration on a reaction product to obtain a dark brown precipitate, washing the dark brown precipitate with the deionized water and absolute ethyl alcohol, and drying to obtain a layered double-magnetic metal hydroxide precursor;
2) the preparation of the magnetic metal @ carbon composite wave-absorbing material comprises the following steps:
placing the layered double-magnetic metal hydroxide precursor prepared in the step 1) into a tubular furnace, introducing protective atmosphere Ar, heating the tubular furnace to 500-900 ℃ at the speed of 1-10 ℃/min, and calcining for 1-4h to prepare the magnetic metal @ carbon composite wave-absorbing material derived from the layered double-magnetic metal hydroxide.
2. The preparation method of the layered double magnetic metal hydroxide derived magnetic metal @ carbon composite wave-absorbing material as claimed in claim 1, wherein in the step 1), the mass ratio of the magnetic metal source, urea and glucose is (2-6): (6-10): (1-4).
3. The method for preparing the layered double magnetic metal hydroxide derived magnetic metal @ carbon composite wave-absorbing material as claimed in claim 1, wherein in the step 1), the magnetic metal source is any two of a divalent nickel ion compound, a trivalent iron ion compound and a divalent cobalt ion compound.
4. The preparation method of the layered double magnetic metal hydroxide derived magnetic metal @ carbon composite wave-absorbing material as claimed in claim 3, wherein the divalent nickel ion compound is any one of nickel nitrate, nickel chloride and nickel sulfate.
5. The preparation method of the layered double magnetic metal hydroxide derived magnetic metal @ carbon composite wave-absorbing material according to claim 3, wherein the ferric ion compound is any one of ferric nitrate, ferric chloride and ferric sulfate.
6. The preparation method of the layered double magnetic metal hydroxide derived magnetic metal @ carbon composite wave-absorbing material as claimed in claim 3, wherein the divalent cobalt ion compound is any one of cobalt nitrate, cobalt chloride and cobalt sulfate.
7. The preparation method of the layered double magnetic metal hydroxide derived magnetic metal @ carbon composite wave-absorbing material as claimed in claim 1, wherein in the step 1), the washing is performed for 3 to 6 times.
8. The preparation method of the layered double magnetic metal hydroxide derived magnetic metal @ carbon composite wave-absorbing material according to claim 1, wherein in the step 1), the drying is carried out at a temperature of 60-90 ℃ for 12-24 hours.
9. A magnetic metal @ carbon composite wave-absorbing material derived from the layered double-magnetic metal hydroxide prepared by the preparation method of any one of claims 1-8.
10. The application of the magnetic metal @ carbon composite material as defined in any one of claims 1-8 in the field of wave-absorbing materials.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116282221A (en) * | 2023-03-06 | 2023-06-23 | 西北大学 | ZIF-67 modified NiFe-LDH wave-absorbing material, preparation method and application |
| CN116828835A (en) * | 2023-08-30 | 2023-09-29 | 四川农业大学 | Carbon-based spiral hollow heterogeneous composite material and preparation method and application thereof |
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2022
- 2022-05-05 CN CN202210480636.5A patent/CN114845538A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116282221A (en) * | 2023-03-06 | 2023-06-23 | 西北大学 | ZIF-67 modified NiFe-LDH wave-absorbing material, preparation method and application |
| CN116828835A (en) * | 2023-08-30 | 2023-09-29 | 四川农业大学 | Carbon-based spiral hollow heterogeneous composite material and preparation method and application thereof |
| CN116828835B (en) * | 2023-08-30 | 2023-11-24 | 四川农业大学 | Carbon-based spiral hollow heterogeneous composite material and preparation method and application thereof |
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