CN112321990B - Preparation method of molybdenum diselenide and carbon nano tube composite wave-absorbing material - Google Patents
Preparation method of molybdenum diselenide and carbon nano tube composite wave-absorbing material Download PDFInfo
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- CN112321990B CN112321990B CN202011257389.XA CN202011257389A CN112321990B CN 112321990 B CN112321990 B CN 112321990B CN 202011257389 A CN202011257389 A CN 202011257389A CN 112321990 B CN112321990 B CN 112321990B
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Abstract
A preparation method of a molybdenum diselenide and carbon nanotube composite wave-absorbing material comprises the steps of fully dissolving purified carbon nanotubes, potassium selenocyanate and ammonium molybdate tetrahydrate in water and ethylene glycol, adding the solution into a stainless steel high-pressure reaction kettle, preparing the molybdenum diselenide and carbon nanotube composite material by a one-step solvothermal method, melting epoxy resin by heat, mixing the epoxy resin with the composite material, and cooling to obtain the molybdenum diselenide and carbon nanotube composite wave-absorbing material. The method has the advantages of simple preparation process and low experimental cost, and the prepared wave-absorbing material has small density, light weight, wide wave-absorbing frequency band and strong wave-absorbing performance, can be used as a light wave-absorbing structure material, a wave-absorbing coating, a wave-absorbing filling material and the like, and can be widely applied to the fields of electromagnetic wave absorption, stealth technology, electromagnetic shielding and the like.
Description
Technical Field
The invention relates to the field of wave-absorbing materials, in particular to a preparation method of a molybdenum diselenide and carbon nano tube composite wave-absorbing material.
Background
The development of stealth technology makes the research on the electromagnetic wave absorbing material more urgent day by day, whether the electromagnetic wave can effectively enter the wave absorbing material and reach high absorption needs to meet impedance matching and attenuation characteristics, the wave absorbing material can be divided into a dielectric medium type and a magnetic medium type according to a loss mechanism, and a typical magnetic medium type wave absorbing material comprises materials such as ferrite, carbonyl iron and the like, but the ferrite has high density and cannot meet the characteristic of low density of the wave absorbing material.
The invention provides a molybdenum diselenide and carbon nanotube composite wave-absorbing material based on a carbon material, which realizes a ferroelectric wave-absorbing material by controlling the conductivity of the composite material by controlling the doping amount of the molybdenum diselenide and has the outstanding advantages of low density, large specific surface area and the like. Meanwhile, the conductivity and the magnetic conductivity of the material are comprehensively regulated and controlled by further doping a small amount of magnetic media such as ferrite, and the excellent composite wave-absorbing material with wider effective absorption frequency band, thinner material thickness, lighter material quality and stronger mechanical property can be prepared.
Disclosure of Invention
The invention aims to provide a preparation method of an effective composite wave-absorbing material based on a carbon material for meeting the characteristic of low density of the wave-absorbing material, so that the composite wave-absorbing material of molybdenum diselenide and carbon nano tubes is obtained, has the advantages of wide absorption frequency band, strong wave-absorbing performance and simple preparation process, and can be widely applied to the fields of light wave-absorbing structure materials, wave-absorbing coatings, wave-absorbing filling materials and the like.
The above purpose is realized by the following technical scheme: and mixing the purified carbon nano tube with a selenium source and a molybdenum source, adding the mixture into a stainless steel high-pressure reaction kettle, preparing a composite material of molybdenum diselenide and the carbon nano tube by a one-step solvothermal method, mixing hot melting epoxy resin and the composite material, and cooling to obtain the composite wave-absorbing material of the molybdenum diselenide and the carbon nano tube. The specific steps of the scheme are as follows:
(1) carrying out ultrasonic treatment on a mixed solution of carbon nano tubes and dilute nitric acid (30%), then filtering and washing with water until the solution is neutral, and drying in vacuum to obtain purified carbon nano tubes;
(2) adding purified carbon nano tubes, ammonium molybdate tetrahydrate, potassium selenocyanate and polyvinylpyrrolidone (PVP) powder serving as a reactive agent into a mixed solution of water and ethylene glycol, and stirring by ultrasound and magnetic force to fully dissolve;
(3) transferring the mixed solution into a stainless steel high-pressure reaction kettle, carrying out solvothermal reaction in a vacuum drying oven, washing with water and absolute ethyl alcohol to remove impurities after the solvothermal reaction is finished, and carrying out vacuum drying to obtain a composite material powder sample of molybdenum diselenide and carbon nano tubes;
(4) heating the epoxy resin to heat and melt, stirring and fully mixing the epoxy resin with the molybdenum diselenide and carbon nano tube composite material, adding the epoxy resin curing agent, and cooling to prepare the molybdenum diselenide and carbon nano tube composite wave-absorbing material.
The addition amount of the carbon nano tube in the step (1) is 100-500mg, and the addition amount of the dilute nitric acid is 100-500 ml.
The ultrasonic time in the step (1) is 3-6h, the vacuum drying temperature is 50-60 ℃, and the vacuum drying time is 6-24 h.
The addition amount of the purified carbon nano tube in the step (2) is 500mg, the addition amount of the ammonium molybdate tetrahydrate is 0.071-0.286mmol, the addition amount of the potassium selenocyanate is 1-4mmol, and the addition amount of the reactive agent is 100 mg-400 mg.
The molar ratio of the molybdenum source to the selenium source in the step (2) is 1: 14, the water is preferably deionized water or ultrapure water, and the volume ratio of the water to the glycol is 1: 1.
The ultrasonic and magnetic stirring time in the step (2) is 30-120 min.
The solvent thermal reaction temperature in the step (3) is 200-220 ℃, the reaction time is 22-24h, the volume ratio of the added mixed solution to the polytetrafluoroethylene lining volume is about 80%, the vacuum drying temperature is 50-60 ℃, and the vacuum drying time is 6-24 h.
The epoxy resin curing agent in the step (4) is ethylenediamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine and diethylaminopropylamine.
The mass ratio of the epoxy resin, the epoxy resin curing agent and the molybdenum diselenide to carbon nano tube composite material in the step (4) is 3: 1: 0.1-0.3.
Compared with the prior art, the invention has the technical effects that:
(1) the light composite wave-absorbing material with low density is prepared by combining a semiconductor and a carbon material, and has the advantages of low material density, light weight, corrosion resistance, simple and convenient use and strong wave-absorbing performance.
(2) The preparation process is simple, the experiment cost is low, and the conductivity and the magnetic conductivity of the material can be comprehensively regulated and controlled by doping a small amount of magnetic media such as ferrite, so that the wave-absorbing performance of the material is further enhanced.
(3) The synergistic effect between the different scale structures of the molybdenum diselenide nanosheets and the carbon nanotubes can effectively enhance the conductance loss and the polarization relaxation loss of the material, increase the dielectric loss capacity of the material and improve the absorption performance of electromagnetic waves.
(4) Further, the composite wave-absorbing film material of molybdenum diselenide and carbon nano tubes can be prepared on a silicon carbide substrate, an alloy plate, a titanium plate or an aluminum plate by a spraying method, a spin-coating method, a dripping method or a brush-coating method.
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FIG. 1 is a flow chart of the preparation of the molybdenum diselenide and carbon nanotube composite wave-absorbing material.
Detailed Description
For better understanding of the present invention, the technical solution of the present invention will be described in detail below by using examples, but the scope of the present invention to be claimed is not limited to the following examples. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Example 1
The method comprises the steps of carrying out ultrasonic treatment on a mixed solution of 100mg of carbon nanotubes and 100ml of dilute nitric acid (30%) for 3 hours, filtering and washing the mixed solution by deionized water until the solution is neutral, drying the mixed solution at 50 ℃ in vacuum for 12 hours to obtain purified carbon nanotubes, adding 100mg of the purified carbon nanotubes, 0.071mmol of ammonium molybdate tetrahydrate, 1mmol of potassium selenocyanate and 100mg of polyvinylpyrrolidone into a mixed solution of 80ml of ultrapure water and ethylene glycol, and carrying out ultrasonic and magnetic stirring for 60 minutes to fully dissolve the mixture.
And transferring the mixed solution into a 100ml polytetrafluoroethylene lining, putting the lining into a stainless steel high-pressure reaction kettle, reacting at the high temperature of 200 ℃ for 24h, cleaning the black product with deionized water and absolute ethyl alcohol for 3 times to remove impurities after the reaction is finished, and drying at the temperature of 50 ℃ in vacuum for 12h to obtain the composite material of molybdenum diselenide and the carbon nano tube.
Heating 6g of epoxy resin to be hot-melted, stirring and fully mixing the epoxy resin with the composite material of molybdenum diselenide and carbon nano tubes, adding 2g of epoxy resin curing agent ethylenediamine, and cooling to prepare the molybdenum diselenide and carbon nano tube composite wave-absorbing material.
Example 2
The method comprises the steps of carrying out ultrasonic treatment on a mixed solution of 200mg of carbon nanotubes and 200ml of dilute nitric acid (30%) for 3 hours, filtering and washing the mixed solution by deionized water until the solution is neutral, drying the mixed solution at the temperature of 60 ℃ in vacuum for 12 hours to obtain purified carbon nanotubes, adding the mixed solution of 200mg of purified carbon nanotubes, 0.071mmol of ammonium molybdate tetrahydrate, 1mmol of potassium selenocyanate and 120mg of polyvinylpyrrolidone into a mixed solution of 80ml of ultrapure water and ethylene glycol, and carrying out ultrasonic and magnetic stirring for 60 minutes to fully dissolve the mixture.
And transferring the mixed solution into a 100ml polytetrafluoroethylene lining, putting the lining into a stainless steel high-pressure reaction kettle, reacting at the high temperature of 210 ℃ for 22h, cleaning the black product with deionized water and absolute ethyl alcohol for 3 times to remove impurities after the reaction is finished, and drying at the temperature of 50 ℃ in vacuum for 12h to obtain the composite material of molybdenum diselenide and the carbon nano tube.
Heating 4.8g of epoxy resin to be hot-melted, stirring and fully mixing the epoxy resin with the composite material of molybdenum diselenide and carbon nano tubes, adding 1.6g of epoxy resin curing agent hexamethylenediamine, and cooling to prepare the molybdenum diselenide and carbon nano tube composite wave-absorbing material.
Example 3
The method comprises the steps of carrying out ultrasonic treatment on a mixed solution of 300mg of carbon nanotubes and 300ml of dilute nitric acid (30%) for 4 hours, filtering and washing the mixed solution by deionized water until the solution is neutral, drying the mixed solution at 50 ℃ in vacuum for 16 hours to obtain purified carbon nanotubes, adding 300mg of the purified carbon nanotubes, 0.143mmol of ammonium molybdate tetrahydrate, 2mmol of potassium selenocyanate and 200mg of polyvinylpyrrolidone into a mixed solution of 100ml of ultrapure water and ethylene glycol, and carrying out ultrasonic and magnetic stirring for 60 minutes to fully dissolve the mixture.
And transferring the mixed solution into a 120ml polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a stainless steel high-pressure reaction kettle, reacting for 24 hours at the high temperature of 210 ℃, cleaning the black product for 3 times by using deionized water and absolute ethyl alcohol after the reaction is finished to remove impurities, and drying for 24 hours at the temperature of 60 ℃ in vacuum to obtain the composite material of molybdenum diselenide and carbon nano tubes.
Heating 9g of epoxy resin to be hot-melted, stirring and fully mixing with the composite material of molybdenum diselenide and carbon nano tubes, adding 3g of epoxy resin curing agent diethylenetriamine, and cooling to prepare the composite wave-absorbing material of molybdenum diselenide and carbon nano tubes.
Example 4
The method comprises the following steps of carrying out ultrasonic treatment on a mixed solution of 400mg of carbon nanotubes and 400ml of dilute nitric acid (30%) for 5 hours, filtering and washing the mixed solution by deionized water until the solution is neutral, drying the mixed solution at the temperature of 60 ℃ in vacuum for 18 hours to obtain purified carbon nanotubes, adding 400mg of the purified carbon nanotubes, 0.143mmol of ammonium molybdate tetrahydrate, 2mmol of potassium selenocyanate and 210mg of polyvinylpyrrolidone into a mixed solution of 100ml of ultrapure water and ethylene glycol, and carrying out ultrasonic and magnetic stirring for 90 minutes to fully dissolve the mixture.
And transferring the mixed solution into a 120ml polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a stainless steel high-pressure reaction kettle, reacting at 220 ℃ for 23h, cleaning a black product for 3 times by using deionized water and absolute ethyl alcohol after the reaction is finished to remove impurities, and drying at 60 ℃ in vacuum for 24h to obtain the composite material of molybdenum diselenide and the carbon nano tube.
Heating 7.2g of epoxy resin to be hot-melted, stirring and fully mixing the epoxy resin with the composite material of molybdenum diselenide and carbon nano tubes, adding 2.4g of epoxy resin curing agent triethylene tetramine, and cooling to prepare the molybdenum diselenide and carbon nano tube composite wave-absorbing material.
Example 5
The method comprises the following steps of carrying out ultrasonic treatment on a mixed solution of 500mg of carbon nanotubes and 500ml of dilute nitric acid (30%) for 6 hours, filtering and washing the mixed solution by deionized water until the solution is neutral, drying the mixed solution at the temperature of 60 ℃ in vacuum for 24 hours to obtain purified carbon nanotubes, adding 500mg of the purified carbon nanotubes, 0.286mmol of ammonium molybdate tetrahydrate, 4mmol of potassium selenocyanate and 400mg of polyvinylpyrrolidone into a mixed solution of 160ml of ultrapure water and ethylene glycol, and carrying out ultrasonic and magnetic stirring for 120 minutes to fully dissolve the mixture.
Transferring the mixed solution into a 200ml polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a stainless steel high-pressure reaction kettle, reacting for 24 hours at a high temperature of 220 ℃, cleaning the black product for 3 times by using deionized water and absolute ethyl alcohol after the reaction is finished to remove impurities, and then drying for 24 hours at a temperature of 60 ℃ in vacuum to obtain the composite material of molybdenum diselenide and carbon nano tubes.
Heating 24.9g of epoxy resin to be hot-melted, fully mixing the epoxy resin with the composite material of the molybdenum diselenide and the carbon nano tube, adding 8.3g of epoxy resin curing agent diethylaminopropylamine, and then cooling to prepare the molybdenum diselenide and carbon nano tube composite wave-absorbing material.
Claims (4)
1. A preparation method of molybdenum diselenide and carbon nano tube composite wave-absorbing material is characterized by comprising the following steps:
(1) carrying out ultrasonic treatment on the carbon nano tube and a dilute nitric acid mixed solution with the concentration of 30%, then filtering and washing with water until the solution is neutral, and carrying out vacuum drying to obtain a purified carbon nano tube;
(2) dissolving purified carbon nano tubes, ammonium molybdate tetrahydrate, potassium selenocyanate and polyvinylpyrrolidone powder in a mixed solution of water and ethylene glycol, and stirring by ultrasonic waves and magnetic forces to fully dissolve;
(3) transferring the mixed solution into a stainless steel high-pressure reaction kettle, carrying out solvothermal reaction in a vacuum drying oven, washing with water and absolute ethyl alcohol to remove impurities after the solvothermal reaction is finished, and carrying out vacuum drying to obtain a composite material powder sample of molybdenum diselenide and carbon nano tubes;
(4) heating epoxy resin to be hot-melted, stirring and fully mixing the epoxy resin with the composite material of molybdenum diselenide and carbon nano tubes, adding an epoxy resin curing agent, and cooling to prepare the molybdenum diselenide and carbon nano tube composite wave-absorbing material; the mass ratio of the epoxy resin, the epoxy resin curing agent and the molybdenum diselenide to carbon nano tube composite material is 3: 1: 0.1-0.3.
2. The method as claimed in claim 1, wherein the amount of the purified carbon nanotubes is 100-500 mg.
3. The method of claim 1, wherein the molar ratio of ammonium molybdate tetrahydrate to potassium selenocyanate is 1: 14.
4. The method as claimed in claim 1, wherein the solvothermal reaction temperature is 200-220 ℃ and the reaction time is 22-24 h.
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| CN114634795B (en) * | 2022-03-25 | 2023-07-18 | 哈尔滨师范大学 | Preparation method of vanadium diselenide/CNTs composite material with full-band and multiband electromagnetic wave absorption performance |
| CN116925497A (en) * | 2023-07-21 | 2023-10-24 | 广州润泰新材料科技有限公司 | Novel fireproof material and preparation method and application thereof |
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