CN115915738A - HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite material and preparation method thereof - Google Patents

HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite material and preparation method thereof Download PDF

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CN115915738A
CN115915738A CN202211107173.4A CN202211107173A CN115915738A CN 115915738 A CN115915738 A CN 115915738A CN 202211107173 A CN202211107173 A CN 202211107173A CN 115915738 A CN115915738 A CN 115915738A
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dimensional
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何建平
潘俊杰
王涛
杨玲
曲宏娇
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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Abstract

The invention discloses a HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite material and a preparation method thereof, belonging to the field of electromagnetic wave absorbing materials. The electromagnetic wave absorbing material with multiple loss characteristics is prepared by a solvothermal method and high-temperature thermal reduction in an inert atmosphere, the magnetic loss capacity of the material is effectively improved by doping Ni nano particles, the wave impedance matching characteristic of the whole material is improved, a multistage nanotube structure is generated by generating a Ni-based coordination compound, favorable conditions are provided for realizing multiple scattering of electromagnetic waves, excellent electromagnetic wave absorbing performance is shown, the minimum reflectivity can reach-50.4 dB and the effective wave absorbing frequency bandwidth can reach 7.32GHz under the condition that the thickness is 2.95mm, and the mass ratio of a wave absorbing agent in a coating is only 10 wt.%.

Description

HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of electromagnetic wave absorbing materials, and particularly relates to a HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite wave absorbing material and a preparation method thereof.
Background
The rapid development of modern electromagnetic communication technology, such as the successive research and development and application of 4G and 5G devices and the wide use of various electronic products in daily life, enables people to be in a complicated electromagnetic pollution environment all the time, and seriously affects the health of people; meanwhile, the use of various precision electronic devices also requires effective solution of the problem of electromagnetic compatibility due to a complicated electromagnetic environment. At present, the application of electromagnetic wave absorption and shielding materials becomes a main means for effectively solving various electromagnetic pollution and electromagnetic compatibility problems, and meanwhile, the design of light-weight, strong-absorption, broadband and thin-thickness wave-absorbing materials becomes a difficult point for scientific research personnel to attack science and technology.
The design of the carbon-based wave absorbing material is an effective method for preparing the lightweight wave absorbing agent, and the macro porous structure and the micro low-dimensional design are the main implementation means at present. For example, the application of low-dimensional carbon materials such as graphene and carbon nanotubes, the design of the honeycomb-structure-type wave-absorbing material and the like can effectively achieve the application goal of lightening the wave-absorbing material. However, the application of a single carbon wave-absorbing material often brings about the disadvantages of large coating thickness, narrow effective wave-absorbing frequency bandwidth and the like. In order to overcome the defects of the application of a single carbon material, an effective method is provided for uniformly loading a magnetic wave-absorbing material on a carbon material framework. The Chenping topic group of university of major continental engineering develops a high-performance magnetic graphene aerogel nanocomposite material (Synthesis of magnetic graphene aerogels for microwave absorption by a in-situ pyrolysis, carbon, 2019-05-01) with low density and enhanced microwave absorption performance for the first time through a two-step strategy of combining hydrothermal reaction and in-situ pyrolysis; the co-doped Ni-Zn ferrite is loaded on the surface of graphene by one-pot hydrothermal method by combining the Yao Nangjun subject group of Nanjing aerospace university and the Nanyang university, and both surfaces of the graphene sheet are densely covered by ferrite nanoparticles. Electromagnetic properties indicate that the content of graphene plays an important role in determining the dielectric properties and magnetic anisotropy of carbon Materials, which further affects the impedance matching and attenuation capabilities of the absorber (Small magnetic Co-doped NiZn ferrite/graphene nanocomposites and the dual-region microwave absorption performance, journal of Materials Chemistry C, 2016-09-23). Although these methods are effective in improving the magnetic loss capability of the material, how to ensure uniform dispersion of the magnetic nanoparticles in the carbon framework remains a difficult problem to effectively solve.
Hydrogen-bonded organic framework materials (HOFs) are special porous crystalline materials with high porosity and high specific surface area, and are mainly formed by intermolecular hydrogen bonding self-assembly between organic building units. The method has the advantages of mild synthesis conditions, high crystallinity, large specific surface area and the like, so that the method has wide application prospect. However, the weak strength of hydrogen bonds in HOFs makes their structures less stable, inevitably leading to structural collapse under high temperature conditions. In order to improve the structural stability of HOFs, commonly used effective methods include pi-pi stacking, H-bond interpenetration, electrostatic attraction, post-synthesis modification, and the like. These methods can effectively improve the structural stability of HOFs, but the relatively single electromagnetic wave attenuation capability seriously hinders the improvement of the electromagnetic wave absorption performance. Therefore, the introduction of the magnetic material to improve the wave-absorbing performance under the premise of ensuring the structural stability of the HOF material is an urgent problem to be solved.
Disclosure of Invention
The invention provides an HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material and a preparation method thereof, wherein the wave-absorbing material still has the characteristics of strong absorption and broadband of electromagnetic waves under low filling degree, and shows excellent electromagnetic wave absorption performance; the preparation method has low cost and simple process, and can be used for large-scale industrial production.
In order to solve the technical problems, the invention adopts the following technical scheme:
an HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material is characterized in that the structure of an electromagnetic wave-absorbing agent is a one-dimensional nano hollow tubular structure and uniformly distributed Ni nano particles. The one-dimensional hollow tubular structure is multi-interface, and metal Ni is uniformly distributed in the whole carbon skeleton; the method is beneficial to improving the multiple loss capability of the material, increasing the multiple scattering effect of the electromagnetic waves in the material and optimizing the wave impedance matching of the material.
Wherein the pipe diameter of the hollow tubular structure is not more than 100nm, and the Ni nano-particles are uniformly distributed in the whole carbon skeleton.
The preparation method of the HOF derived one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material comprises the following steps:
step 1: dissolving 1.2mmol (0.1513 g) of melamine in 35mL of methanol solution, magnetically stirring for 10min, and then dissolving 1.2mmol (0.2522 g) of trimesic acid in the solution and keeping stirring for 30min; thereafter, 1.2mmol (0.3489 g) of nickel nitrate hexahydrate (Ni (NO) 3 ) 2 ·6H 2 O) dissolving in the solution, and continuing to magnetically stir for 10min;
wherein the mol ratio of melamine, trimesic acid and nickel nitrate hexahydrate is 1:1:1;
wherein, the stirring is carried out at room temperature (20-30 ℃);
step 2: transferring the mixed solution into a 50ml reaction kettle for solvothermal reaction at the temperature of 150 ℃ for 12 hours, and after the reaction kettle is naturally cooled to the room temperature, performing subsequent centrifugation, washing and drying on the solvothermal product to obtain Ni 2+ A doped HOF precursor product;
wherein the volume of the mixed solution in the reaction kettle accounts for 70 percent;
wherein, the solution used for centrifuging and washing the solvent thermal product is methanol;
and step 3: mixing Ni 2+ And calcining the doped HOF precursor product in a nitrogen atmosphere, setting the heating rate to be 2 ℃/min, the heat treatment temperature to be 600-900 ℃, and keeping the temperature for 2h to finally obtain the one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material.
Has the beneficial effects that: the invention provides an HOF derived one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material and a preparation method thereofForming a hydrogen bond organic framework with a one-dimensional nanorod structure at the temperature; by introducing Ni 2+ The complex reacts with melamine and trimesic acid under the condition of solvothermal reaction, and the original hydrogen bond functional groups are partially destroyed, so that a hollow tubular structure is generated; meanwhile, the structural stability of the original HOF material is greatly improved due to the generation of coordination bonds, the magnetic loss capacity of the material is effectively improved due to the doping of Ni nano particles, the integral wave impedance matching characteristic of the material is also improved, and in addition, favorable conditions are provided for realizing multiple scattering of electromagnetic waves due to the generation of Ni-based coordination compounds. Compared with the traditional microwave absorbent, the wave-absorbing material prepared by the invention has the characteristics of wide effective absorption frequency band, strong wave-absorbing capability and light weight under extremely low filling degree, and has excellent electromagnetic wave absorption performance; meanwhile, the preparation method does not need complex synthesis equipment, has simple process and low cost, and is suitable for large-scale industrial production.
Drawings
FIG. 1 is an SEM image of a HOF precursor product obtained by liquid-phase stirring at room temperature in examples 1, 2, 3 and 4 of the present invention;
FIG. 2 shows Ni prepared in examples 1, 2, 3 and 4 of the present invention 2+ SEM pictures of doped HOF precursor products;
FIG. 3 is an SEM photograph of Ni @ CNT-600 produced in example 1 of the present invention;
FIG. 4 is an SEM photograph of Ni @ CNT-700 produced in example 2 of the present invention;
FIG. 5 is an SEM photograph of Ni @ CNT-800 produced in example 3 of the present invention;
FIG. 6 is an SEM photograph of Ni @ CNT-900 produced in example 4 of the present invention;
FIG. 7 shows Ni obtained in examples 1, 2, 3 and 4 of the present invention 2+ FTIR plot of doped HOF precursor product;
FIG. 8 shows Ni prepared in examples 1, 2, 3 and 4 of the present invention 2+ TGA profile of the doped HOF precursor product;
FIG. 9 is an XRD pattern of Ni @ CNT-600, ni @ CNT-700, ni @ CNT-800 and Ni @ CNT-900 produced in examples 1, 2, 3 and 4 of the present invention;
FIG. 10 is an electrical loss factor graph of Ni @ CNT-600, ni @ CNT-700, ni @ CNT-800, and Ni @ CNT-900 according to examples 1, 2, 3, and 4 of the present invention;
FIG. 11 is a graph of magnetic loss factors of Ni @ CNT-600, ni @ CNT-700, ni @ CNT-800 and Ni @ CNT-900 produced in examples 1, 2, 3 and 4 of the present invention;
FIG. 12 is a graph of reflection loss for Ni @ CNT-600 produced in example 1 of the present invention;
FIG. 13 is a graph of the reflection loss of Ni @ CNT-700 produced in example 2 of the present invention;
FIG. 14 is a graph of reflection loss for Ni @ CNT-800 produced in example 3 of the present invention;
FIG. 15 is a graph of the reflection loss of Ni @ CNT-900 produced in example 4 of the present invention;
FIG. 16 is a schematic view of the principle of the preparation method of the present invention.
Detailed Description
The invention is described in detail below with reference to the following figures and specific examples:
example 1
A preparation method of a HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material comprises the following steps:
step 1, 1.2mmol (0.1513 g) of melamine was dissolved in 35mL of methanol solution, magnetically stirred for 10min, and then 1.2mmol (0.2522 g) of trimesic acid was dissolved in the above solution and kept stirring for 30min. Thereafter, 1.2mmol (0.3489 g) of nickel nitrate hexahydrate (Ni (NO) 3 ) 2 ·6H 2 O) dissolving in the solution, and continuing to magnetically stir for 10min;
step 2, transferring the mixed solution into a 50ml reaction kettle for solvothermal reaction at 150 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and then performing subsequent centrifugation, methanol washing and drying on the solvothermal product to obtain Ni 2+ A doped HOF precursor product;
step 3, adding Ni 2+ And calcining the doped HOF precursor product in a nitrogen atmosphere, setting the heating rate to be 2 ℃/min, the heat treatment temperature to be 600 ℃, and the heat preservation time to be 2h, thereby finally obtaining the one-dimensional Ni-doped magnetic carbon-based nanocomposite Ni @ CNT-600.
Example 2
A preparation method of a HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material comprises the following steps:
step 1, 1.2mmol (0.1513 g) of melamine was dissolved in 35mL of methanol solution, magnetically stirred for 10min, and then 1.2mmol (0.2522 g) of trimesic acid was dissolved in the above solution and kept stirring for 30min. Thereafter, 1.2mmol (0.3489 g) of nickel nitrate hexahydrate (Ni (NO) 3 ) 2 ·6H 2 O) dissolving in the solution, and continuing to magnetically stir for 10min;
step 2, transferring the mixed solution into a 50ml reaction kettle for solvothermal reaction at the temperature of 150 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and then performing subsequent centrifugation, methanol washing and drying on the solvothermal product to obtain Ni 2+ A doped HOF precursor product;
step 3, adding Ni 2+ And calcining the doped HOF precursor product in a nitrogen atmosphere, setting the heating rate to be 2 ℃/min, the heat treatment temperature to be 700 ℃, and the heat preservation time to be 2h, thereby finally obtaining the one-dimensional Ni-doped magnetic carbon-based nanocomposite Ni @ CNT-700.
Example 3
A preparation method of a HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material comprises the following steps:
step 1, 1.2mmol (0.1513 g) of melamine was dissolved in 35mL of methanol solution, magnetically stirred for 10min, and then 1.2mmol (0.2522 g) of trimesic acid was dissolved in the above solution and kept stirring for 30min. Thereafter, 1.2mmol (0.3489 g) of nickel nitrate hexahydrate (Ni (NO) 3 ) 2 ·6H 2 O) dissolving in the solution, and continuing to magnetically stir for 10min;
step 2, transferring the mixed solution into a 50ml reaction kettle for solvothermal reaction at the temperature of 150 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and then performing subsequent centrifugation, methanol washing and drying on the solvothermal product to obtain Ni 2+ A doped HOF precursor product;
step 3, adding Ni 2+ Doped HOF precursor products inCalcining in nitrogen atmosphere, setting the heating rate at 2 ℃/min, the heat treatment temperature at 800 ℃ and the heat preservation time at 2h, and finally obtaining the one-dimensional Ni-doped magnetic carbon-based nanocomposite Ni @ CNT-800.
Example 4
A preparation method of a HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material comprises the following steps:
step 1, 1.2mmol (0.1513 g) of melamine was dissolved in 35mL of methanol solution, magnetically stirred for 10min, and then 1.2mmol (0.2522 g) of trimesic acid was dissolved in the above solution and kept stirring for 30min. Thereafter, 1.2mmol (0.3489 g) of nickel nitrate hexahydrate (Ni (NO) 3 ) 2 ·6H 2 O) dissolving in the solution, and continuing to magnetically stir for 10min;
step 2, transferring the mixed solution into a 50ml reaction kettle for solvothermal reaction at the temperature of 150 ℃ for 12 hours, naturally cooling the reaction kettle to room temperature, and then performing subsequent centrifugation, methanol washing and drying on the solvothermal product to obtain Ni 2+ A doped HOF precursor product;
step 3, adding Ni 2+ And calcining the doped HOF precursor product in a nitrogen atmosphere, setting the heating rate to be 2 ℃/min, the heat treatment temperature to be 900 ℃, and the heat preservation time to be 2h, thereby finally obtaining the one-dimensional Ni-doped magnetic carbon-based nanocomposite Ni @ CNT-900.
FIG. 1 is an SEM image of HOF precursor products prepared by liquid-phase stirring at room temperature in examples 1, 2, 3 and 4 of the present invention. As can be seen from FIG. 1, the HOF precursor product prepared by liquid phase stirring presents a one-dimensional nanorod structure, and the diameter of the HOF precursor product is more than 100nm.
FIG. 2 shows Ni prepared in examples 1, 2, 3 and 4 of the present invention 2+ SEM image of doped HOF precursor product. As can be seen from FIG. 2, ni 2+ The doped HOF precursor product presents a non-uniform one-dimensional hollow nano-tubular structure, and the diameter of the doped HOF precursor product is more than 100nm.
FIG. 3 is an SEM photograph of Ni @ CNT-600 produced in example 1 of the present invention. As can be seen from FIG. 3, the original hollow nanotube-shaped structure is still perfectly maintained by Ni @ CNT-600 after high-temperature calcination at 600 ℃.
FIG. 4 is an SEM photograph of Ni @ CNT-700 obtained in example 2 of the present invention. As can be seen from FIG. 4, the original hollow nanotube-shaped structure is still perfectly maintained by Ni @ CNT-700 after high-temperature calcination at 700 ℃.
FIG. 5 is an SEM photograph of Ni @ CNT-800 obtained in example 3 of the present invention. As can be seen from FIG. 5, the original hollow nanotube-shaped structure of Ni @ CNT-800 is perfectly maintained after the calcination at the high temperature of 800 ℃.
FIG. 6 is an SEM photograph of Ni @ CNT-900 according to example 4 of the present invention. As can be seen from FIG. 6, the original hollow nanotube-shaped structure is perfectly maintained by Ni @ CNT-900 after high temperature calcination at 900 ℃.
FIG. 7 shows Ni obtained in examples 1, 2, 3 and 4 of the present invention 2+ FTIR plot of doped HOF precursor product. As can be seen from FIG. 7, in the hydrogen bonding zone (4000-2500 cm) -1 ) About 3391, 3224 and 3109cm -1 The absorption peaks at (A) correspond to stretching vibration of the secondary amide N-H bond, stretching vibration of the hydroxyl group O-H bond, and stretching vibration of the aromatic ring C-H bond, respectively. Notably, broadening of the absorption peaks for the N-H and O-H bonds indicates that these molecules form a coherent state due to the presence of hydrogen bonds. Furthermore, about 1699cm -1 The absorption peak at (A) corresponds to stretching vibration (amide I peak) of secondary amide C = O bond, and is about 1651cm -1 The absorption peak at (A) corresponds to the bending vibration of the secondary amide N-H bond (amide I peak), about 1326cm -1 The absorption peak at the position corresponds to the stretching vibration of the secondary amide C-N bond (amide I peak); the result shows that the melamine and the trimesic acid have amidation reaction, and the formed covalent bond modification is favorable for the generation of chemical crosslinking effect, so that the structural stability of the HOF material is improved.
FIG. 8 shows Ni obtained in examples 1, 2, 3 and 4 of the present invention 2+ TGA profile of doped HOF precursor product. As can be seen from fig. 8, the weight loss from room temperature to 250 ℃ (17%) is due to the removal of hydrogen bonded water molecules; the weight loss from 250 to 750 ℃ (67.9%) was attributed to the removal of oxygen-containing functional groups and to the pyrolysis and graphitization of the carbon backbone; after exceeding 750 ℃, ni 2+ The weight of the doped HOF precursor product is no longer lost and the pyrolysis process is complete.
FIG. 9 shows the results obtained in examples 1, 2, 3 and 4 of the present inventionXRD patterns of Ni @ CNT-600, ni @ CNT-700, ni @ CNT-800 and Ni @ CNT-900. As can be seen from fig. 9, as the temperature increases, the (1 0) crystal plane diffraction peak of the graphitized carbon gradually becomes sharp from broad to slow, indicating that the graphitization degree of the sample gradually increases. Secondly, the 2 θ diffraction peaks at about 44.5 °, 51.8 ° and 76.4 ° correspond to the (1 1), (2 0) and (2 0) crystal planes of cubic Ni; XRD diffraction peaks of ferromagnetic Ni indicate that Ni is present when the heat treatment temperature is higher than 600 deg.C 2+ Can be completely reduced into a metal elementary substance state.
FIG. 10 is an electrical loss factor graph of Ni @ CNT-600, ni @ CNT-700, ni @ CNT-800, and Ni @ CNT-900 produced in examples 1, 2, 3, and 4 of the present invention. As can be seen from FIG. 10, ni @ CNT-600 possesses relatively weakest electrical loss capability, while Ni @ CNT-900 possesses the largest electrical loss factor and strongest electrical loss capability, which mainly depends on the change of the graphitization degree of the material in the high-temperature carbonization process; while the electrical loss capacity of Ni @ CNT-700 is slightly higher than that of Ni @ CNT-800 because the calcination product at 800 ℃ undergoes a certain degree of structural disruption, thus reducing the electrical loss capacity of the material.
FIG. 11 is a graph showing the magnetic loss factors of Ni @ CNT-600, ni @ CNT-700, ni @ CNT-800 and Ni @ CNT-900 produced in examples 1, 2, 3 and 4 of the present invention. As can be seen from FIG. 11, ni @ CNT-600, ni @ CNT-700 and Ni @ CNT-800 have similar magnetic loss capabilities, which indicates that the heat treatment temperature has little effect on the change of the magnetic properties of the material; the magnetic loss capacity of the Ni @ CNT-900 is reduced, mainly because the one-dimensional nanotube structure is partially collapsed in the heat treatment process, so that the magnetic loss capacity of the material is reduced.
The filling amount of the wave-absorbing material in the paraffin base is 10wt.%, and the wave-absorbing capability is tested, and the result is as follows:
FIG. 12 is a graph showing reflection loss of Ni @ CNT-600 according to example 1 of the present invention. As can be seen from FIG. 12, ni @ CNT-600 has no effective wave-absorbing property in the range of 8-18 GHz.
FIG. 13 is a graph of the reflection loss of Ni @ CNT-700 produced in example 2 of the present invention. As can be seen from FIG. 13, ni @ CNT-700 exhibited excellent electromagnetic wave absorption properties in the Ku band. When the thickness is 2.95mm, the minimum reflectivity can reach-54 dB, and the effective wave-absorbing frequency bandwidth can reach 7.32GHz (10.64-17.96 GHz).
FIG. 14 is a graph of reflection loss of Ni @ CNT-800 produced in example 3 of the present invention. As can be seen from FIG. 14, ni @ CNT-800 also exhibits good electromagnetic wave absorption properties in the Ku band. When the thickness is 2.4mm, the minimum reflectivity can reach-56.9 dB, and the effective wave-absorbing frequency bandwidth can reach 5.95GHz (12.05-18 GHz).
FIG. 15 is a graph of reflection loss of Ni @ CNT-900 produced in example 4 of the present invention. As can be seen from FIG. 15, ni @ CNT-900 exhibits poor wave-absorbing performance in the range of 8-18GHz, and the wave-absorbing performance is far inferior to Ni @ CNT-700 and Ni @ CNT-800.
The wave absorbing principle of the Ni-doped magnetic carbon-based nanotube composite wave absorbing material derived from the one-dimensional HOF is as follows: first, by introducing Ni 2+ The coordination reaction is carried out with melamine and trimesic acid, so that a hollow tubular structure is generated; multiple scattering and absorption of electromagnetic waves in the material are effectively increased; meanwhile, the Ni magnetic metal nanoparticles are uniformly dispersed in the carbon skeleton, so that the magnetic loss capacity of the material is effectively improved, and the wave impedance matching characteristic of the material is effectively regulated and controlled. Therefore, the one-dimensional Ni-doped magnetic carbon-based nanotube composite material synthesized by the invention has excellent electromagnetic wave absorption performance.
The above description is only a preferred embodiment of the present invention, and it is obvious to those skilled in the art that various changes and modifications can be made based on the above technical solutions and concepts, and all such changes and modifications should be included in the protection scope of the present invention.

Claims (7)

1. An HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material is characterized in that the wave-absorbing material is in a one-dimensional nano hollow tubular structure and uniformly distributed Ni nano particles; the one-dimensional nano hollow tubular structure is a multi-interface, and the Ni nano particles are uniformly distributed in the whole carbon skeleton.
2. The HOF-derived one-dimensional Ni-doped magnetic carbon-based nanocomposite wave-absorbing material as claimed in claim 1, wherein the tube diameter of the one-dimensional nano hollow tubular structure is not more than 100nm.
3. A preparation method of a HOF derived one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material is characterized by comprising the following steps:
step 1: dissolving melamine in a methanol solution, uniformly stirring, dissolving trimesic acid in the solution, and keeping stirring to form a hydrogen bond organic framework;
step 2: dissolving nickel nitrate hexahydrate in the solution obtained in the step (1), and continuously stirring; then carrying out solvothermal reaction, ni 2+ Performing coordination reaction with melamine and trimesic acid under the condition of solvothermal reaction, naturally cooling to room temperature after the reaction is finished, and performing subsequent centrifugation, washing and drying on the product to obtain Ni 2+ A doped HOF precursor product;
and 3, step 3: ni obtained in step 2 2+ And calcining the doped HOF precursor product in a nitrogen atmosphere to obtain the one-dimensional Ni-doped magnetic carbon-based nano composite wave-absorbing material.
4. The method for preparing the HOF-derived one-dimensional Ni-doped magnetic carbon-based nanocomposite wave-absorbing material according to claim 3, wherein the step 1 is performed at room temperature.
5. The method for preparing the HOF-derived one-dimensional Ni-doped magnetic carbon-based nanocomposite wave-absorbing material according to claim 3 or 4, wherein the molar ratio of the melamine, the trimesic acid and the nickel nitrate hexahydrate is 1:1:1.
6. the method for preparing the HOF-derived one-dimensional Ni-doped magnetic carbon-based nanocomposite wave-absorbing material according to claim 3, wherein the reaction temperature of the solvothermal reaction in the step 2 is 150 ℃ and the reaction time is 12 h.
7. The method for preparing the HOF-derived one-dimensional Ni-doped magnetic carbon-based nanocomposite wave-absorbing material according to claim 3, wherein the temperature rise rate of calcination in the step 3 is 2 ℃/min, the temperature is 600-900 ℃, and the heat preservation time is 2 h.
CN202211107173.4A 2022-09-09 2022-09-09 HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite material and preparation method thereof Pending CN115915738A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117463342A (en) * 2023-12-27 2024-01-30 山东海化集团有限公司 Preparation method of porous hollow tubular heterojunction catalyst for electrolyzing seawater and oxygen evolution application of porous hollow tubular heterojunction catalyst
CN117463373A (en) * 2023-12-27 2024-01-30 山东海化集团有限公司 Porous hollow tubular CoS 2 /NiS 2 Rapid preparation method and application of heterojunction

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117463342A (en) * 2023-12-27 2024-01-30 山东海化集团有限公司 Preparation method of porous hollow tubular heterojunction catalyst for electrolyzing seawater and oxygen evolution application of porous hollow tubular heterojunction catalyst
CN117463373A (en) * 2023-12-27 2024-01-30 山东海化集团有限公司 Porous hollow tubular CoS 2 /NiS 2 Rapid preparation method and application of heterojunction
CN117463373B (en) * 2023-12-27 2024-04-05 山东海化集团有限公司 Porous hollow tubular CoS 2 /NiS 2 Rapid preparation method and application of heterojunction
CN117463342B (en) * 2023-12-27 2024-04-05 山东海化集团有限公司 Preparation method of porous hollow tubular heterojunction catalyst for electrolyzing seawater and oxygen evolution application of porous hollow tubular heterojunction catalyst

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