A 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorption material and preparation method
By introducing nickel chains into graphene-based aerogels to grow molybdenum disulfide nanosheets and magnetic metal nickel chains, the conductivity and sheet stacking problems of graphene and molybdenum disulfide absorbing materials are solved, and the electromagnetic wave absorption capacity is significantly improved.
Patent Information
- Application Number
- CN202210740409.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-06-28
- Publication Date
- 2025-07-11
- Estimated Expiration
- 2042-06-28
AI Technical Summary
The existing graphene and molybdenum disulfide absorbing materials have problems such as high conductivity, weak sheet stacking and weak losses in the field of electromagnetic absorption, which hinder their further application.
The nickel chain is used as a carrier to grow molybdenum disulfide nanosheets in situ, and a magnetic metal nickel chain is introduced to recombinate it with reduced graphene oxide aerogel. Through the synergistic effect of magnetic loss and dielectric materials, the graphene sheet layer stacking and dielectric constant are improved and the electromagnetic wave absorption capacity is improved.
The electromagnetic wave absorption capacity is significantly improved, the material preparation is simple and can be produced on a large scale, and the introduction of dielectric/magnetic loss media adjusts the impedance matching characteristics and enhances the attenuation capability.
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Abstract
Description
Technical Field
[0001] The present invention relates to a graphene-based aerogel composite microwave absorbing material, specifically to a 1T / 2H phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorbing material and a preparation method thereof, belonging to the technical field of nanomaterial preparation. Background Art
[0002] With the development of modern electronic information technology, the popularization of various electronic and electrical equipment, intelligent devices, and the wide use of mobile communication devices, while people enjoy great convenience in daily life, it has also brought serious electromagnetic pollution to the environment in which humans live. A series of environmental and social problems caused by electromagnetic pollution have begun to be concerned by people. To avoid secondary pollution, the development and research of microwave absorbing materials and electromagnetic shielding materials mainly based on absorption have become one of the effective protection means.
[0003] Graphene has been widely used in various scientific research and industrial fields due to its large specific surface area, rich active sites, excellent electrical conductivity, etc. In particular, graphene-based aerogels have advantages such as a three-dimensional network structure, low density, high porosity, and high specific surface area, making them show great advantages in the field of microwave absorbing materials. As a typical two-dimensional transition metal dichalcogenide, molybdenum disulfide (MoS₂) is composed of three layers of atoms of S-Mo-S, and different polycrystalline structures (mainly three types: 1T, 2H, and 3R) can be formed according to different coordination modes and / or interlayer stacking orders between transition metal and chalcogen element atoms, showing unique electrical and optical properties. In the field of electromagnetic attenuation, it shows good attenuation performance. In particular, the octahedrally coordinated metal 1T phase shows unique physical and chemical properties, such as faster electron and charge injection / transfer, enlarged interlayer spacing, and increased active sites on the basal plane and edges, making it show potential advantages in electromagnetic wave absorption. However, single graphene absorbents have disadvantages such as high electrical conductivity, weak sheet stacking and loss; while single MoS₂ absorbents still have problems such as inherent low electrical conductivity and few polarization active sites, which hinder their further application in the field of electromagnetic wave absorption.
[0004] Therefore, it is of great practical significance and application prospect to seek a graphene-based aerogel absorbent material with simple process operation and excellent microwave absorbing performance. Summary of the Invention
[0005] The object of the present invention is to overcome the problems existing in the prior art and provide a 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite wave-absorbing material and a preparation method thereof. Molybdenum disulfide nanosheets are in-situ grown with nickel chains as carriers, and magnetic metal nickel chains are introduced to enhance the magnetic loss of the system. Together with the dielectric material molybdenum disulfide, the problems of graphene sheet stacking, large dielectric constant, and impedance mismatch are synergistically improved, the attenuation ability of the system is enhanced, and the electromagnetic wave absorption ability is significantly improved.
[0006] To achieve the above object, the present invention adopts the following technical solutions: A preparation method of a 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite wave-absorbing material, comprising the following preparation steps:
[0007] S1. Preparation of metal nickel chains: The nickel salt precursor is dispersed in an ethylene glycol solution, and then sodium hydroxide and hydrazine hydrate are successively added to the above solution and stirred evenly by magnetic stirring. The reaction is carried out under a water bath condition to prepare magnetic metal nickel chains;
[0008] S2. Preparation of 1T / 2H-phase molybdenum disulfide and nickel chain composite: The magnetic metal nickel chains prepared in the above step S1 are added to the precursor solutions of the molybdenum source and the sulfur source according to a mass ratio, a reducing agent is added, and ultrasonic treatment is carried out to disperse evenly. The reaction is carried out under hydrothermal conditions to prepare a 1T / 2H-phase molybdenum disulfide@nickel chain composite;
[0009] S3. Preparation of the composite wave-absorbing material: The 1T / 2H-phase molybdenum disulfide@nickel chain composite prepared in the above step S2 and the graphene oxide solution are magnetically stirred and mixed at room temperature according to a mass ratio, and the reaction is carried out under hydrothermal conditions to finally prepare a 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite wave-absorbing material.
[0010] In the above step S1, the nickel salt precursor includes nickel chloride, nickel nitrate, nickel sulfate, nickel bromide, and nickel hydroxide.
[0011] In the above step S1, the water bath reaction temperature is 60~90°C, and the water bath reaction time is 0.5~3h; the magnetic stirring time is 15min.
[0012] In the above step S2, the precursor solutions of the molybdenum source and the sulfur source include ammonium tetrathiomolybdate, molybdenum trioxide and thioacetamide, molybdenum trioxide and potassium thiocyanate, sodium molybdate and thioacetamide, sodium molybdate and thiourea, and ammonium molybdate and thiourea.
[0013] In the above step S2, the solvent of the precursor solutions of the molybdenum source and the sulfur source is N,N-dimethylformamide; the reducing agent is hydrazine hydrate.
[0014] In the step S2, the mass ratio of the magnetic metal nickel chain to the molybdenum source solution is 1-8:1.
[0015] In the step S2, the time of the ultrasonic treatment is 20-60 min; the hydrothermal reaction temperature is 160-220 °C, and the hydrothermal reaction time is 8-12 h.
[0016] In the step S3, the mass concentration of the graphene oxide solution is 5 mg / ml, and the addition amount of the 1T / 2H phase molybdenum disulfide@nickel chain composite is 5-30 wt% of the mass of the graphene oxide solution.
[0017] In the step S3, the time for magnetically stirring and mixing the 1T / 2H phase molybdenum disulfide@nickel chain composite and the graphene oxide solution is 1 h; the hydrothermal reaction temperature is 140-200 °C, and the hydrothermal reaction time is 6-10 h.
[0018] The present invention protects the 1T / 2H phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorbing material prepared according to the method.
[0019] The beneficial effects of the present invention are as follows:
[0020] 1) In the preparation method of the present invention, molybdenum disulfide nanosheets are in-situ grown with nickel chains as carriers. The magnetic field effect of the metal nickel chains themselves can induce partial phase transformation of molybdenum disulfide. The large number of introduced 1T / 2H interfaces promotes the dipole distribution dynamics, and the presence of the metal-semiconductor hybrid phase enhances the electron transfer ability.
[0021] 2) In the preparation method of the present invention, the raw materials are cheap and easily available, the operation process is simple, and large-scale preparation can be carried out; at the same time, the introduction of the dielectric / magnetic loss medium effectively adjusts the impedance matching characteristics and attenuation ability of the material system, making it have good application prospects in the field of electromagnetic microwave absorbing materials.
[0022] 3) In the composite microwave absorbing material prepared by the present invention, the introduction of magnetic metal nickel chains enhances the magnetic loss of the system, and together with the dielectric material molybdenum disulfide, it collaboratively improves problems such as graphene sheet stacking, large dielectric constant, and impedance mismatch, improves the attenuation ability of the system, and significantly improves the electromagnetic wave absorption ability. Description of the Drawings
[0023] Figure 1 It is the scanning electron microscope image of the 1T / 2H-MoS2@Ni chain after hydrothermal reaction in Example 1 of the present invention;
[0024] Figure 2 It is the scanning electron microscope image of the 1T / 2H-MoS2@Ni chain / rGO aerogel after hydrothermal reaction in Example 1 of the present invention;
[0025] Figure 3 X-ray diffraction pattern of 1T / 2H-MoS2@Ni chain / rGO aerogel after hydrothermal reaction in Example 1 of the present invention;
[0026] Figure 4 Electromagnetic wave absorption performance diagram of 1T / 2H-MoS2@Ni chain / rGO aerogel after hydrothermal reaction in Example 1 of the present invention;
[0027] Figure 5 Optimal electromagnetic wave absorption performance comparison diagram of 1T / 2H-MoS2@Ni chain / rGO aerogel after hydrothermal reaction in Examples 1-6 of the present invention. Detailed implementation manners
[0028] The present invention will be further explained below with reference to the accompanying drawings and specific embodiments.
[0029] Example 1: A preparation method of a 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite wave-absorbing material, comprising the following preparation steps:
[0030] S1. Preparation of metallic nickel chains: Disperse 1.2 g of nickel chloride in 100 ml of ethylene glycol solution, then sequentially add 1.7 g of sodium hydroxide and 5 ml of hydrazine hydrate to the above solution, mix evenly by magnetic stirring for 15 min, react at 80 °C under water bath conditions for 1 h, take the precipitate after the reaction, and prepare magnetic metallic nickel chains after repeated washing and drying;
[0031] S2. Preparation of 1T / 2H-phase molybdenum disulfide and nickel chain complex: Add 40 mg of ammonium tetrathiomolybdate to 60 ml of N,N-dimethylformamide solution, ultrasonically disperse evenly, add 160 mg of nickel chains, continue ultrasonic dispersion, add 200 μl of hydrazine hydrate, continue ultrasonic dispersion for 30 min, transfer to a 100 ml hydrothermal reaction kettle, react at 200 °C under water bath conditions for 10 h, take the precipitate after the reaction, and prepare 1T / 2H-phase molybdenum disulfide@nickel chain complex after repeated washing and drying;
[0032] S3. Preparation of the composite wave-absorbing material: Disperse the 1T / 2H-phase molybdenum disulfide@nickel chain complex in 10 ml of deionized water according to 10 wt% of the mass of the graphene oxide solution, ultrasonically disperse evenly, mix with 40 ml of graphene oxide solution (mass concentration of 5 mg / ml), magnetically stir at room temperature for 1 h, transfer to a 100 ml hydrothermal reaction kettle, react at 180 °C under water bath conditions for 8 h, take the precipitate after the reaction, and finally prepare the 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite wave-absorbing material after repeated washing and drying.
[0033] Example 2: A preparation method of 1T / 2H phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorption material, comprising the following preparation steps:
[0034] S1. Preparation of metal nickel chain: Disperse 1.2 g of nickel chloride in 100 ml of ethylene glycol solution, then sequentially add 1.7 g of sodium hydroxide and 5 ml of hydrazine hydrate to the above solution, mix evenly by magnetic stirring for 15 min, react at 60 °C under water bath conditions for 3 h, take the precipitate after the reaction, and prepare magnetic metal nickel chain after repeated washing and drying;
[0035] S2. Preparation of 1T / 2H phase molybdenum disulfide and nickel chain composite: Add 40 mg of ammonium tetrathiomolybdate to 60 ml of N,N-dimethylformamide solution, ultrasonically disperse evenly, add 40 mg of nickel chain, continue ultrasonic dispersion, add 200 μl of hydrazine hydrate, continue ultrasonic dispersion for 30 min, transfer to a 100 ml hydrothermal reaction kettle, react at 160 °C under water bath conditions for 12 h, take the precipitate after the reaction, and prepare 1T / 2H phase molybdenum disulfide@nickel chain composite after repeated washing and drying;
[0036] S3. Preparation of composite microwave absorption material: Disperse the 1T / 2H phase molybdenum disulfide@nickel chain composite in 10 ml of deionized water according to 5 wt% of the mass of the graphene oxide solution, ultrasonically disperse evenly, mix with 40 ml of graphene oxide solution (mass concentration is 5 mg / ml), stir magnetically at room temperature for 1 h, transfer to a 100 ml hydrothermal reaction kettle, react at 140 °C under water bath conditions for 10 h, take the precipitate after the reaction, and finally prepare 1T / 2H phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorption material after repeated washing and drying.
[0037] Example 3: A preparation method of 1T / 2H phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorption material, comprising the following preparation steps:
[0038] S1. Preparation of metal nickel chain: Disperse 1.2 g of nickel chloride in 100 ml of ethylene glycol solution, then sequentially add 1.7 g of sodium hydroxide and 5 ml of hydrazine hydrate to the above solution, mix evenly by magnetic stirring for 15 min, react at 90 °C under water bath conditions for 0.5 h, take the precipitate after the reaction, and prepare magnetic metal nickel chain after repeated washing and drying;
[0039] S2. Preparation of 1T / 2H-phase molybdenum disulfide and nickel chain complex: Add 40 mg of ammonium tetrathiomolybdate to 60 ml of N,N-dimethylformamide solution, ultrasonically disperse it evenly, add 320 mg of nickel chains, continue ultrasonic dispersion, add 200 μl of hydrazine hydrate, continue ultrasonic dispersion for 30 min, transfer it into a 100 ml hydrothermal reaction kettle, react at 220 °C under water bath conditions for 8 h, take the precipitate after the reaction, and prepare 1T / 2H-phase molybdenum disulfide@nickel chain complex after repeated washing and drying;
[0040] S3. Preparation of composite microwave absorbing material: Disperse 1T / 2H-phase molybdenum disulfide@nickel chain complex in 10 ml of deionized water according to 15 wt% of the mass of graphene oxide solution, ultrasonically disperse it evenly, mix it with 40 ml of graphene oxide solution (mass concentration is 5 mg / ml), stir magnetically at room temperature for 1 h, transfer it into a 100 ml hydrothermal reaction kettle, react at 200 °C under water bath conditions for 6 h, take the precipitate after the reaction, and finally prepare 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorbing material after repeated washing and drying.
[0041] Example 4: A preparation method of 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorbing material, including the following preparation steps:
[0042] S1. Preparation of metal nickel chains: Disperse 1.2 g of nickel chloride in 100 ml of ethylene glycol solution, then add 1.7 g of sodium hydroxide and 5 ml of hydrazine hydrate to the above solution in sequence, mix evenly by magnetic stirring for 15 min, react at 80 °C under water bath conditions for 1.5 h, take the precipitate after the reaction, and prepare magnetic metal nickel chains after repeated washing and drying;
[0043] S2. Preparation of 1T / 2H-phase molybdenum disulfide and nickel chain complex: Add 40 mg of ammonium tetrathiomolybdate to 60 ml of N,N-dimethylformamide solution, ultrasonically disperse it evenly, add 80 mg of nickel chains, continue ultrasonic dispersion, add 200 μl of hydrazine hydrate, continue ultrasonic dispersion for 30 min, transfer it into a 100 ml hydrothermal reaction kettle, react at 180 °C under water bath conditions for 9 h, take the precipitate after the reaction, and prepare 1T / 2H-phase molybdenum disulfide@nickel chain complex after repeated washing and drying;
[0044] S3. Preparation of the composite microwave absorbing material: Dispersing the 1T / 2H-phase molybdenum disulfide@nickel chain composite at 20 wt% of the mass of the graphene oxide solution into 10 ml of deionized water, ultrasonically dispersing it evenly, mixing it with 40 ml of graphene oxide solution (mass concentration is 5 mg / ml), magnetically stirring for 1 h at room temperature, transferring it into a 100-ml hydrothermal reaction kettle, reacting for 9 h under the condition of 160 °C water bath. After the reaction, taking the precipitate, washing and drying it repeatedly, and finally preparing the 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorbing material.
[0045] Example 5: A preparation method of a 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorbing material, comprising the following preparation steps:
[0046] S1. Preparation of the metallic nickel chain: Dissolving 1.2 g of nickel chloride in 100 ml of ethylene glycol solution, then adding 1.7 g of sodium hydroxide and 5 ml of hydrazine hydrate into the above solution in sequence, mixing evenly by magnetic stirring for 15 min, reacting for 2.5 h under the condition of 70 °C water bath. After the reaction, taking the precipitate, washing and drying it repeatedly to prepare the magnetic metallic nickel chain;
[0047] S2. Preparation of the 1T / 2H-phase molybdenum disulfide and nickel chain composite: Adding 40 mg of ammonium tetrathiomolybdate into 60 ml of N,N-dimethylformamide solution, ultrasonically dispersing it evenly, adding 240 mg of nickel chain, continuing ultrasonic dispersion, adding 200 μl of hydrazine hydrate, continuing ultrasonic dispersion for 30 min, transferring it into a 100-ml hydrothermal reaction kettle, reacting for 8 h under the condition of 190 °C water bath. After the reaction, taking the precipitate, washing and drying it repeatedly to prepare the 1T / 2H-phase molybdenum disulfide@nickel chain composite;
[0048] S3. Preparation of the composite microwave absorbing material: Dispersing the 1T / 2H-phase molybdenum disulfide@nickel chain composite at 30 wt% of the mass of the graphene oxide solution into 10 ml of deionized water, ultrasonically dispersing it evenly, mixing it with 40 ml of graphene oxide solution (mass concentration is 5 mg / ml), magnetically stirring for 1 h at room temperature, transferring it into a 100-ml hydrothermal reaction kettle, reacting for 8 h under the condition of 190 °C water bath. After the reaction, taking the precipitate, washing and drying it repeatedly, and finally preparing the 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorbing material.
[0049] Example 6: A preparation method of a 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorbing material, comprising the following preparation steps:
[0050] S1. Preparation of metallic nickel chains: 1.2 g of nickel chloride was dispersed in 100 ml of ethylene glycol solution, and then 1.7 g of sodium hydroxide and 5 ml of hydrazine hydrate were successively added to the above solution. After mixing evenly by magnetic stirring for 15 min, the reaction was carried out for 2 h under the condition of 80 °C water bath. After the reaction, the precipitate was taken, and the magnetic metallic nickel chains were prepared after repeated washing and drying;
[0051] S2. Preparation of 1T / 2H-phase molybdenum disulfide and nickel chain composite: 40 mg of ammonium tetrathiomolybdate was added to 60 ml of N,N-dimethylformamide solution, ultrasonically dispersed evenly, 40 mg of nickel chains were added, and ultrasonic dispersion was continued. Then 200 μl of hydrazine hydrate was added, and ultrasonic dispersion was continued for 30 min. The mixture was transferred into a 100 ml hydrothermal reaction kettle, and the reaction was carried out for 8 h under the condition of 210 °C water bath. After the reaction, the precipitate was taken, and the 1T / 2H-phase molybdenum disulfide@nickel chain composite was prepared after repeated washing and drying;
[0052] S3. Preparation of composite microwave absorbing material: The 1T / 2H-phase molybdenum disulfide@nickel chain composite was dispersed into 10 ml of deionized water according to 25 wt% of the mass of the graphene oxide solution, ultrasonically dispersed evenly, and mixed with 40 ml of graphene oxide solution (mass concentration of 5 mg / ml). After magnetic stirring at room temperature for 1 h, the mixture was transferred into a 100 ml hydrothermal reaction kettle, and the reaction was carried out for 9 h under the condition of 170 °C water bath. After the reaction, the precipitate was taken, and the 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite microwave absorbing material was finally prepared after repeated washing and drying.
[0053] The sample of the 1T / 2H-phase molybdenum disulfide@nickel chain composite obtained by the above water bath and hydrothermal reaction was adhered to the conductive adhesive and characterized by a scanning electron microscope, as shown in Figure 1 shown; The 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel sample finally obtained after hydrothermal treatment was adhered to the conductive adhesive and characterized by a scanning electron microscope, as shown in Figure 2 shown; The finally obtained 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel was characterized by an X-ray diffraction pattern, as shown in Figure 3 shown.
[0054] Figure 4Shown are the electromagnetic wave absorption performance graphs of the 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel, molybdenum disulfide / reduced graphene oxide aerogel, and nickel chain / reduced graphene oxide aerogel prepared in Example 1. It can be seen from the results that the wave absorption performance of Example 1 is significantly better than that of the molybdenum disulfide / reduced graphene oxide aerogel and the nickel chain / reduced graphene oxide aerogel. Moreover, the minimum reflection loss value of the material prepared in Example 1 is -51.0 dB at a matching thickness of 2 mm and a frequency of 15.27 GHz, indicating that the constructed 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel has stronger wave absorption performance.
[0055] Figure 5 Shown is the comparison graph of the optimal electromagnetic wave absorption performance of the 1T / 2H-MoS2@Ni chain / rGO aerogel after hydrothermal reaction in Examples 1-6 of the present invention. It can be seen from the results that the optimal reflection loss values of the 1T / 2H-MoS2@Ni chain / rGO aerogel prepared under these conditions are all less than -20 dB, indicating that more than 99% of the electromagnetic wave energy is effectively absorbed at this time. It can be seen that the electromagnetic wave absorption performance under the conditions of Example 1 is the strongest, indicating that there is an optimal ratio of dielectric and magnetic loss media in the material system, and the hydrothermal reaction temperature and time have a greater impact on the performance of the system.
[0056] The 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite wave-absorbing material provided by the present invention realizes the effective generation of magnetic metal nickel chains under the condition of water bath heating, and realizes the partial transformation of semiconductor-phase molybdenum disulfide to 1T / 2H-phase molybdenum disulfide by means of the induction of magnetic metal nickel chains under the condition of hydrothermal reaction; under the action of hydrothermal reduction, graphene oxide is partially reduced, and 1T / 2H-MoS2@Ni chains are uniformly dispersed inside the porous reduced graphene oxide to obtain the 1T / 2H-MoS2@Ni chain / rGO aerogel composite wave-absorbing material.
[0057] In the preparation method of the present invention, molybdenum disulfide nanosheets are in-situ grown with nickel chains as the carrier, and magnetic metal nickel chains are introduced to enhance the magnetic loss of the system. Together with the dielectric material molybdenum disulfide, it synergistically improves the problems of graphene sheet stacking, large dielectric constant, and impedance mismatch, improves the attenuation ability of the system, and significantly improves the electromagnetic wave absorption ability.
[0058] As mentioned above, it is only used to illustrate the technical solution of the present invention and not to limit it. Other modifications or equivalent replacements made by those of ordinary skill in the art to the technical solution of the present invention should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solution of the present invention.
Claims
1. Preparation method of 1T / 2H-phase molybdenum disulfide @ nickel chain / reduced graphene oxide aerogel composite microwave absorption material, characterized by comprising: It includes the following preparation steps: S1. Preparation of metallic nickel chains: Disperse a nickel salt precursor in an ethylene glycol solution, then successively add sodium hydroxide and hydrazine hydrate to the above solution and stir evenly by magnetic force, and carry out a reaction under a water bath condition to prepare magnetic metallic nickel chains; S2. Preparation of 1T / 2H-phase molybdenum disulfide and nickel chain composite: Add the magnetic metallic nickel chains obtained in the above step S1 to the precursor solution of a molybdenum source and a sulfur source according to a mass ratio, add a reducing agent, disperse evenly by ultrasonic treatment, and carry out a reaction under a hydrothermal condition to prepare a 1T / 2H-phase molybdenum disulfide@nickel chain composite; The mass ratio of the magnetic metallic nickel chains to the molybdenum source solution is 1-8:1; S3. Preparation of a composite absorbing material: Mix the 1T / 2H-phase molybdenum disulfide@nickel chain composite obtained in the above step S2 with a graphene oxide solution according to a mass ratio and stir magnetically at room temperature, and carry out a reaction under a hydrothermal condition to finally prepare a 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite absorbing material.
2. The preparation method of a 1T / 2H-phase molybdenum disulfide @ nickel chain / reduced graphene oxide aerogel composite microwave absorbing material according to claim 1, characterized in that: In the above step S1, the nickel salt precursor includes nickel chloride, nickel nitrate, nickel sulfate, nickel bromide, and nickel hydroxide.
3. The preparation method of a 1T / 2H phase molybdenum disulfide @ nickel chain / reduced graphene oxide aerogel composite microwave absorption material according to claim 1, characterized in that: In the above step S1, the water bath reaction temperature is 60-90°C, and the water bath reaction time is 0.5-3 h; the magnetic stirring time is 15 min.
4. The preparation method of a 1T / 2H-phase molybdenum disulfide @ nickel chain / reduced graphene oxide aerogel composite microwave absorption material according to claim 1, characterized in that: In the above step S2, the molybdenum source and sulfur source precursor solution includes ammonium tetrathiomolybdate, molybdenum trioxide and thioacetamide, molybdenum trioxide and potassium thiocyanate, sodium molybdate and thioacetamide, sodium molybdate and thiourea, and ammonium molybdate and thiourea.
5. The preparation method of a 1T / 2H-phase molybdenum disulfide @ nickel chain / reduced graphene oxide aerogel composite microwave absorption material according to claim 4, characterized in that: In the above step S2, the solvent of the molybdenum source and sulfur source precursor solution is N,N-dimethylformamide; the reducing agent is hydrazine hydrate.
6. The preparation method of a 1T / 2H-phase molybdenum disulfide @ nickel chain / reduced graphene oxide aerogel composite microwave absorption material according to claim 1, characterized in that: In the above step S2, the ultrasonic treatment time is 20-60 min; the hydrothermal reaction temperature is 160-220°C, and the hydrothermal reaction time is 8-12 h.
7. The preparation method of a 1T / 2H phase molybdenum disulfide @ nickel chain / reduced graphene oxide aerogel composite microwave absorption material according to claim 1, characterized in that: In the above step S3, the mass concentration of the graphene oxide solution is 5 mg / ml, and the addition amount of the 1T / 2H-phase molybdenum disulfide@nickel chain composite is 5-30 wt% of the mass of the graphene oxide solution.
8. The preparation method of a 1T / 2H-phase molybdenum disulfide @ nickel chain / reduced graphene oxide aerogel composite microwave absorption material according to claim 1, characterized in that: In the above step S3, the magnetic stirring mixing time of the 1T / 2H-phase molybdenum disulfide@nickel chain composite and the graphene oxide solution is 1 h; the hydrothermal reaction temperature is 140-200°C, and the hydrothermal reaction time is 6-10 h. A 1T / 2H-phase molybdenum disulfide@nickel chain / reduced graphene oxide aerogel composite absorbing material prepared by the method according to any one of claims 1-8.
Citation Information
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