CN111534278A - Preparation method of carbon nano tube composite wave-absorbing material - Google Patents
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Abstract
The invention discloses a preparation method of a carbon nano tube composite wave-absorbing material, which comprises the following steps: (1) ferrite Dy0.4Ni0.4Fe2O4Preparation of (2) pretreatment of carbon nanotubes, (3) preparation of the ferrite Dy0.4Ni0.4Fe2O4Respectively adding the particles and the pretreated carbon nano tube into an ethylene glycol solution, then adding a surfactant, fully stirring, adding an ammonium persulfate solution, carrying out hydrothermal reaction for 3-5h, then centrifuging, washing with deionized water to be neutral, and drying to obtain Dy0.4Ni0.4Fe2O4the/CNTs composite wave-absorbing material. The ultrasonic oscillation of the carbon nano tube in the mixed acid removes the impure carbon; the ferrite nano-particles and the pretreated carbon nano-tubes are added into the ethylene glycol solution to realize the dispersion of the particles, and the addition of the surfactant CTAB/CTAC enables the ferrite nano-particles and the pretreated carbon nano-tubes to be better dispersed in the ethylene glycol system to avoid the bonding and blocking of the particles; the invention uses ferrite Dy0.4Ni0.4Fe2O4Coated on carbon nanotube to prepare novel Dy0.4Ni0.4Fe2O4the/CNTs composite wave-absorbing material.
Description
Technical Field
The invention belongs to the technical field of carbon nano tubes, and particularly relates to a preparation method of a carbon nano tube composite wave-absorbing material.
Background
At present, with the rapid development of electronic technology, electronic, electrical equipment or other information systems have been widely applied in various fields of daily production and life of people. The wide application and development of electronic equipment bring great convenience to the life of people, and the electromagnetic radiation of the electronic equipment has great influence on the health of human beings and the environment depending on survival. With the development of electronic products towards high frequency, high integration and miniaturization, the problems of electromagnetic compatibility and electromagnetic interference of the electronic products become more and more prominent, and therefore higher requirements are put forward on the electromagnetic noise suppression capability of the wave-absorbing material.
The carbon nanotube has the inherent nature of carbon material, the electric and thermal conductivity of metal material, the heat and corrosion resistance of ceramic material, the knittability of textile fiber and the light weight and easy processing property of polymer material. The carbon nano tube is used as a composite material reinforcement, so that the composite material can show good strength, elasticity, fatigue resistance and isotropy, and the carbon nano tube reinforced composite material brings a leap of the performance of the composite material.
The carbon nano tube is singly used as a microwave absorbent, so that a good wave absorbing effect cannot be achieved, the required comprehensive performance can be obtained only by researching the microwave absorbing mechanism of the carbon nano tube and compounding the carbon nano tube with other materials with different performances, and the efficient and practical microwave absorbing material is prepared.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon nano tube composite wave-absorbing material, which is used for preparing the wave-absorbing material with excellent wave-absorbing performance.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a carbon nano tube composite wave-absorbing material comprises the following steps:
(1) ferrite Dy0.4Ni0.4Fe2O4The preparation of (1): FeCl is added3·6H2O、Ni(NO3)2And Dy2O3According to the formula Dy0.4Ni0.4Fe2O4Adding the mixture into deionized water according to the stoichiometric ratio, stirring, adding an alkali solution to adjust the pH value to 11-12, heating to 90-110 ℃, reacting for 4-6h, cooling to room temperature, carrying out suction filtration, washing with the deionized water to be neutral, drying and grinding to obtain Dy0.4Ni0.4Fe2O4Ferrite nanoparticles;
(2) pretreatment of the carbon nanotubes: heating and calcining a multi-walled carbon nanotube, adding the multi-walled carbon nanotube into mixed acid, performing ultrasonic oscillation for 30-40min, heating to 80-90 ℃, stirring for 3-4h, cooling to room temperature, performing suction filtration, washing to be neutral by using deionized water, drying, and grinding to obtain a pretreated carbon nanotube;
(3) the Dy is reacted with0.4Ni0.4Fe2O4Respectively adding ferrite nano particles and the pretreated carbon nano tube into an ethylene glycol solution, then adding a surfactant, fully stirring, adding an ammonium persulfate solution, carrying out hydrothermal reaction for 3-5h, then centrifuging, washing with deionized water to be neutral, and drying to obtain Dy0.4Ni0.4Fe2O4/CNTs composite nano wave-absorbing material.
Preferably, the alkali solution in the step (1) is one of NaOH and KOH solutions, and the concentration of the alkali solution is 1-2.5 mol/L.
Preferably, the drying temperature in the step (1) is 70-90 ℃, and the drying time is 3-5 h.
Preferably, the drying temperature in the step (2) is 70-90 ℃, and the drying time is 3-5 h.
Preferably, the calcination temperature in the step (2) is 500-550 ℃, and the calcination time is 1-3 h.
Preferably, the mixed acid in the step (2) is prepared by mixing concentrated nitric acid and concentrated sulfuric acid according to the volume ratio of 1: 3.
Preferably, in the step (3), the surfactant is one of cetyltrimethylammonium bromide (CTAB) and cetyltrimethylammonium chloride (CTAC), the concentration of the surfactant in the system after the surfactant is added is 0.05-0.2mol/L, and the concentration of the ammonium persulfate solution in the system after the ammonium persulfate solution is added is 0.2-0.5 mol/L.
The invention calcines the carbon nano tube for 1-3h at the temperature of 500-550 ℃, which aims to remove most amorphous carbon impurities such as amorphous carbon on the surface of the carbon nano tube and achieve the purpose of primary purification of the carbon nano tube.
Ferrite (Dy)0.4Ni0.4Fe2O4) The double-loss wave-absorbing nano material has excellent magnetism and lower electric conductivity, and the surface of the carbon nano tube is uniformly coated with a layer of ferrite nano particles, so that the dielectricity of the carbon nano tube can be effectively reduced, and the carbon nano tube has magnetism, thereby improving the impedance matching of the material and reducing the reflection of electromagnetic waves; on the other hand, the ferrite has magnetic loss, and can enhance the wave-absorbing performance of the material. Thus Dy0.4Ni0.4Fe2O4the/CNTs composite nano wave-absorbing material effectively combines excellent mechanical property, electrical property and thermal stability of the carbon nano tube and Dy of ferrite0.4Ni0.4Fe2O4The nano material has excellent magnetic property and better wave-absorbing property.
Compared with the prior art, the invention has the following beneficial effects: the ultrasonic oscillation of the carbon nano tube in the mixed acid removes the impure carbon; the ferrite nano-particles and the pretreated carbon nano-tubes are added into the ethylene glycol solution to realize the dispersion of the particles, and the addition of the surfactant CTAB/CTAC enables the ferrite nano-particles and the pretreated carbon nano-tubes to be better dispersed in the ethylene glycol system to avoid the bonding and blocking of the particles; the invention uses ferrite Dy0.4Ni0.4Fe2O4Coated on carbon nanotube to prepare novel Dy0.4Ni0.4Fe2O4the/CNTs composite wave-absorbing material.
Detailed Description
The present invention will be further described with reference to examples, but the present invention is not limited to these examples.
The carbon nanotubes used in the examples were multi-walled carbon nanotubes with a purity of greater than 90% and a diameter of 10-30 nm.
Example 1
(1) Ferrite Dy0.4Ni0.4Fe2O4The preparation of (1): FeCl is added3·6H2O、Ni(NO3)2And Dy2O3According to the formula Dy0.4Ni0.4Fe2O4Adding the mixture into deionized water according to the stoichiometric ratio, stirring, adding 1mol/L NaOH solution to adjust the pH to 11, heating to 90 ℃, reacting for 5 hours, cooling to room temperature, carrying out suction filtration, washing with the deionized water to be neutral, drying at 80 ℃ for 4 hours, and grinding to obtain Dy0.4Ni0.4Fe2O4Ferrite nanoparticles;
(2) pretreatment of the carbon nanotubes: heating a multi-walled carbon nanotube to 525 ℃, calcining for 2h, adding mixed acid (prepared by 1:3 volume ratio of concentrated nitric acid to concentrated sulfuric acid) into the mixed acid, ultrasonically oscillating for 35min, heating to 85 ℃, stirring for 3h, cooling to room temperature, carrying out suction filtration, washing to be neutral by deionized water, drying for 4h at 80 ℃, and grinding to obtain a pretreated carbon nanotube;
(3) will be 4gDy0.4Ni0.4Fe2O4Respectively adding ferrite nano particles and 1g of pretreated carbon nano tube into 25g of ethylene glycol solution, then adding a surfactant CTAB (the concentration of the added surfactant in the system is 0.05 mol/L), fully stirring, adding an ammonium persulfate solution (the concentration of the added surfactant in the system is 0.2 mol/L), carrying out hydrothermal reaction for 4h, then centrifuging, washing with deionized water to neutrality, and drying to obtain Dy0.4Ni0.4Fe2O4/CNTs composite nano wave-absorbing material.
The composite wave-absorbing material prepared in the embodiment has a frequency bandwidth of 16.8GHz with a reflectivity loss value lower than-10 dB in 2-18GHz, and a minimum reflectivity loss value of-47.3 dB.
Example 2
(1) Ferrite Dy0.4Ni0.4Fe2O4The preparation of (1): FeCl is added3·6H2O、Ni(NO3)2And Dy2O3According to the formula Dy0.4Ni0.4Fe2O4Adding the mixed solution into deionized water according to the stoichiometric ratio, stirring, adding 1.5mol/L NaOH solution to adjust the pH value to 12, heating to 100 ℃, reacting for 4 hours, cooling to room temperature, performing suction filtration, washing with the deionized water to be neutral, drying for 3 hours at 90 ℃, and grinding to obtain Dy0.4Ni0.4Fe2O4Ferrite nanoparticles;
(2) pretreatment of the carbon nanotubes: heating a multi-walled carbon nanotube to 500 ℃, calcining for 3h, adding mixed acid (prepared by 1:3 volume ratio of concentrated nitric acid to concentrated sulfuric acid) into the mixture, ultrasonically oscillating for 30min, heating to 80 ℃, stirring for 4h, cooling to room temperature, carrying out suction filtration, washing to be neutral by using deionized water, drying for 3h at 90 ℃, and grinding to obtain a pretreated carbon nanotube;
(3) 2gDy0.4Ni0.4Fe2O4Respectively adding ferrite nano particles and 1g of pretreated carbon nano tube into 25g of ethylene glycol solution, then adding a surfactant CTAC (the concentration of the added surfactant in the system is 0.2 mol/L), fully stirring, adding an ammonium persulfate solution (the concentration of the added surfactant in the system is 0.5 mol/L), carrying out hydrothermal reaction for 3h, then centrifuging, washing with deionized water to neutrality, and drying to obtain Dy0.4Ni0.4Fe2O4/CNTs composite nano wave-absorbing material.
The composite wave-absorbing material prepared in the embodiment has a frequency bandwidth of 16.5GHz with a reflectivity loss value lower than-10 dB in 2-18GHz, and a minimum reflectivity loss value of-46.5 dB.
Example 3
(1) Ferrite Dy0.4Ni0.4Fe2O4The preparation of (1): FeCl is added3·6H2O、Ni(NO3)2And Dy2O3According to the formula Dy0.4Ni0.4Fe2O4Adding the mixture into deionized water according to the stoichiometric ratio, stirring, adding 2.5mol/L KOH solution to adjust the pH value to 11, heating to 110 ℃, reacting for 6 hours, cooling to room temperature, carrying out suction filtration, washing to be neutral by the deionized water,drying at 70 ℃ for 5h, and grinding to obtain Dy0.4Ni0.4Fe2O4Ferrite nanoparticles;
(2) pretreatment of the carbon nanotubes: heating a multi-walled carbon nanotube to 550 ℃, calcining for 1h, adding mixed acid (prepared by 1:3 volume ratio of concentrated nitric acid to concentrated sulfuric acid) into the mixture, ultrasonically oscillating for 40min, heating to 90 ℃, stirring for 3h, cooling to room temperature, carrying out suction filtration, washing to be neutral by using deionized water, drying for 5h at 70 ℃, and grinding to obtain a pretreated carbon nanotube;
(3) will be 6gDy0.4Ni0.4Fe2O4Respectively adding ferrite nano particles and 1g of pretreated carbon nano tube into 25g of ethylene glycol solution, then adding a surfactant CTAB (the concentration of the added surfactant in the system is 0.1 mol/L), fully stirring, adding an ammonium persulfate solution (the concentration of the added surfactant in the system is 0.3 mol/L), carrying out hydrothermal reaction for 5h, then centrifuging, washing with deionized water to neutrality, and drying to obtain Dy0.4Ni0.4Fe2O4/CNTs composite nano wave-absorbing material.
The composite wave-absorbing material prepared in the embodiment has the frequency bandwidth of 17.4GHz with the reflectivity loss value lower than-10 dB in 2-18GHz, and the minimum reflectivity loss value can reach-47.5 dB.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention; those skilled in the art can make various changes, modifications and alterations without departing from the scope of the invention, and all equivalent changes, modifications and alterations to the disclosed technology are equivalent embodiments of the present invention; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (7)
1. A preparation method of a carbon nano tube composite wave-absorbing material is characterized by comprising the following steps:
(1) ferrite Dy0.4Ni0.4Fe2O4The preparation of (1): FeCl is added3·6H2O、Ni(NO3)2And Dy2O3According to the formula Dy0.4Ni0.4Fe2O4Adding the mixture into deionized water according to the stoichiometric ratio, stirring, adding an alkali solution to adjust the pH value to 11-12, heating to 90-110 ℃, reacting for 4-6h, cooling to room temperature, carrying out suction filtration, washing with the deionized water to be neutral, drying and grinding to obtain Dy0.4Ni0.4Fe2O4Ferrite nanoparticles;
(2) pretreatment of the carbon nanotubes: heating and calcining a multi-walled carbon nanotube, adding the multi-walled carbon nanotube into mixed acid, performing ultrasonic oscillation for 30-40min, heating to 80-90 ℃, stirring for 3-4h, cooling to room temperature, performing suction filtration, washing to be neutral by using deionized water, drying, and grinding to obtain a pretreated carbon nanotube;
(3) the Dy is reacted with0.4Ni0.4Fe2O4Respectively adding ferrite nano particles and the pretreated carbon nano tube into an ethylene glycol solution, then adding a surfactant, fully stirring, adding an ammonium persulfate solution, carrying out hydrothermal reaction for 3-5h, then centrifuging, washing with deionized water to be neutral, and drying to obtain Dy0.4Ni0.4Fe2O4the/CNTs composite wave-absorbing material.
2. The method for preparing the carbon nano tube composite wave-absorbing material according to claim 1, wherein the alkali solution in the step (1) is one of NaOH and KOH solutions, and the concentration of the alkali solution is 1-2.5 mol/L.
3. The method for preparing the carbon nano tube composite wave-absorbing material according to claim 1, wherein the drying temperature in the step (1) is 70-90 ℃, and the drying time is 3-5 h.
4. The method for preparing the carbon nano tube composite wave-absorbing material according to claim 1, wherein the drying temperature in the step (2) is 70-90 ℃, and the drying time is 3-5 h.
5. The method for preparing the carbon nanotube composite wave-absorbing material as claimed in claim 1, wherein the calcination temperature in the step (2) is 500-550 ℃ and the calcination time is 1-3 h.
6. The method for preparing the carbon nano tube composite wave-absorbing material according to claim 1, wherein the mixed acid in the step (2) is prepared from concentrated nitric acid and concentrated sulfuric acid according to the volume ratio of 1: 3.
7. The method for preparing the carbon nanotube composite wave-absorbing material according to claim 1, wherein the surfactant in the step (3) is one of cetyltrimethylammonium bromide (CTAB) and cetyltrimethylammonium chloride (CTAC), the concentration of the surfactant in the system after the surfactant is added is 0.05-0.2mol/L, and the concentration of the ammonium persulfate solution in the system after the ammonium persulfate solution is added is 0.2-0.5 mol/L.
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| CN115011162A (en) * | 2022-07-21 | 2022-09-06 | 南京信息工程大学 | Attapulgite-reinforced carbon nanotube wave-absorbing material and preparation method thereof |
| CN115228434A (en) * | 2022-07-21 | 2022-10-25 | 南京信息工程大学 | Surface-wrapped gamma-Al 2 O 3 : carbon nanotube adsorbent with Dy & lt 3+ & gt particles and preparation method thereof |
| CN115433549A (en) * | 2022-08-18 | 2022-12-06 | 中国地质大学（武汉） | Composite microsphere with wave absorbing and heat management functions and preparation method and application thereof |
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Application publication date: 20200814 |