CN107325787B - Hollow carbon nano-particles and wave-absorbing material prepared from same - Google Patents
Hollow carbon nano-particles and wave-absorbing material prepared from same Download PDFInfo
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Abstract
The invention provides hollow carbon nano-particles and a wave-absorbing material prepared from the same. The preparation method of the hollow carbon nanoparticles comprises the following steps: mixing aniline, pyrrole, a nonionic surfactant and water to obtain a first solution; adding an ammonium persulfate solution into the first solution after ice bath to obtain a second solution; carrying out suction filtration, washing and freeze drying on the second solution after reaction to obtain a primary product; and carbonizing the primary product to obtain the hollow carbon nano-particles. The preparation method of the wave-absorbing material comprises the following steps: adding graphene, hollow carbon nano particles and polypropylene into a torque rheometer for banburying to obtain a mixture; and carrying out hot pressing and cold pressing on the mixture to obtain the wave-absorbing material. According to the technical scheme provided by the invention, the graphene and the hollow carbon nanoparticles are used as wave-absorbing media, the polypropylene is used as a carrier, and the prepared wave-absorbing material not only can effectively absorb electromagnetic waves, but also integrates a series of advantages of low density, fatigue resistance and the like of the polypropylene material.
Description
Technical Field
The invention relates to hollow carbon nano-particles and a wave-absorbing material prepared from the same, belonging to the technical field of polymer composite materials.
Background
The wave-absorbing material is a material capable of absorbing and attenuating incident electromagnetic waves and converting the incident electromagnetic energy into heat energy to dissipate the energy or eliminate the electromagnetic waves due to interference, is an important functional material, and is widely applied to electronic products, stealth technology, microwave communication, microwave darkroom, electromagnetic radiation resistance, electromagnetic pollution prevention and the like. Therefore, the development of a wave absorbing material is crucial.
In recent years, the demand for wave-absorbing materials is continuously increased, the effect and the position of the electromagnetic wave-absorbing materials are more and more prominent, and the traditional magnetic materials such as ferrite have higher density and are easy to oxidize, so that the significance of developing high-performance composite wave-absorbing materials is great.
In the prior art, the electromagnetic wave-absorbing material is prepared by using graphene mainly through methods such as an oxidation-reduction method and a Chemical Vapor Deposition (CVD) method, however, the method has the defects that mass production cannot be realized or a large amount of pollutants are generated in the preparation process, the requirement of environmental protection and no pollution cannot be met, and mass production cannot be realized in industry.
Therefore, it is an urgent technical problem to be solved in the art to provide a method for preparing a wave-absorbing material, which is simple, easy, green and pollution-free, and can be used in industrial mass production.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide a hollow carbon nanoparticle and a method for preparing the same; the hollow carbon nano-particles provided by the invention have a unique hollow structure, so that incident electromagnetic waves can form multiple reflections in the cavity, and the wave absorbing performance of the wave absorbing material can be greatly improved.
The invention also provides a wave-absorbing material prepared from the hollow carbon nano-particles.
In order to achieve the above object, the present invention provides a method for preparing hollow carbon nanoparticles, comprising the steps of:
mixing aniline, pyrrole, a nonionic surfactant and water to obtain a first solution;
adding an ammonium persulfate solution into the first solution after ice bath to obtain a second solution;
reacting the second solution at 0-5 ℃ for 8-16h, and then performing suction filtration, washing and freeze drying to obtain a primary product;
and carbonizing the primary product to obtain the hollow carbon nano-particles. The hollow carbon nanoparticles have a substantially spherical shape and thus may be referred to as hollow carbon nanoball.
In the above method, preferably, the ratio of the aniline, the pyrrole, the nonionic surfactant and the water is 0.76mL:0.58mL (0.04-0.16) g:120 mL.
In one embodiment, aniline, pyrrole, nonionic surfactant, and water are mixed in an amount of 0.76mL, pyrrole in an amount of 0.58mL, nonionic surfactant in an amount of (0.04-0.16) g, and water in an amount of 120 mL.
In the above method, preferably, the nonionic surfactant is Triton X-100 (the Triton X-100 is also called as emulsifier TX-100, and is also called as Triton X-100).
In the above method, preferably, when aniline, pyrrole, a nonionic surfactant, and water are mixed, the water is deionized water.
In the above method, preferably, the method further comprises the step of stirring, sonicating, and ice-bathing the first solution; more preferably, when the first solution is subjected to ice bath, the temperature of the ice bath is 0-5 ℃, and the time of the ice bath is 30-50 min.
In the above method, preferably, the ammonium persulfate solution is obtained by dissolving ammonium persulfate in deionized water, wherein the ratio of the ammonium persulfate to the water is 3.8g:30 mL.
In the above method, preferably, when the ammonium persulfate solution is subjected to ice bath, the temperature of the ice bath is 0-5 ℃, and the time of the ice bath is 30-50 min.
In the above method, preferably, the washing comprises the following processes: preparing ethanol and water into an ethanol solution according to the volume ratio of 1 (3-5); and washing the solution after the reaction by using the ethanol solution.
In the above method, the temperature of the freeze-drying is generally around 50 ℃ below zero.
In the method, the temperature of the carbonization treatment is preferably 700-900 ℃; more preferably, the atmosphere of the carbonization treatment is nitrogen or argon; further preferably, the temperature increase rate is controlled to 3 ℃/min when the carbonization treatment is performed.
The invention also provides the hollow carbon nano-particles prepared by the method.
In order to achieve the purpose, the invention also provides a preparation method of the wave-absorbing material, which comprises the following steps:
adding graphene, hollow carbon nano particles and polypropylene into a torque rheometer, and banburying at 190-220 ℃ for 10-20min to obtain a mixture;
and hot-pressing the mixture at the temperature of 190 ℃ and 220 ℃ for 5-10min under the pressure of 15-20MPa, and then cold-pressing the mixture at the room temperature and the pressure of 20-25MPa for 5-8min to obtain the wave-absorbing material. The wave-absorbing material is a compound of graphene, hollow carbon nano-particles and polypropylene.
According to the technical scheme provided by the invention, the wave-absorbing material is prepared by taking polypropylene as a carrier and graphene and a hollow carbon nano material as effective wave-absorbing media. The addition of the hollow carbon nano particles can reduce the quality of the compound, and the unique hollow structure of the hollow carbon nano particles can enable incident electromagnetic waves to form multiple reflections in the cavity, so that the wave absorbing performance of the compound is greatly improved on the basis of graphene; in addition, the polypropylene is used as a carrier, so that the prepared wave-absorbing material not only integrates the advantages of small density, fatigue resistance, chemical corrosion resistance, stress cracking resistance, easiness in molding and processing and the like of the polypropylene material, but also plays a role in high value-added utilization of the polypropylene material produced by a refinery.
In the above method, the banburying is one of the main functions of the torque rheometer.
In the above method, preferably, the mass ratio of the graphene, the hollow carbon nanoparticles and the polypropylene is 1 (4-6): 19. Too large mass fraction of graphene can result in too good conductivity of the wave-absorbing material, and increase reflection of electromagnetic waves, thereby being not beneficial to absorption; if the mass ratio is too small, the absorption loss capacity of the wave-absorbing material is insufficient, and the incident electromagnetic waves cannot be effectively absorbed, so that the mass fraction of the graphene powder can be controlled in an optimum range by adopting the mass ratio provided by the invention, and the absorption effect of the electromagnetic waves is ensured; in addition, the quality of the hollow carbon nano particles is controlled to be in the proportion, so that the wave absorbing performance of the material can be greatly improved.
In the method, preferably, the rotating speed of the torque rheometer in the banburying process is 30-50 r/min. The rotation speed can ensure that the graphene and the hollow carbon nanoparticles are uniformly dispersed in the polypropylene, the rotation speed can be adjusted according to the temperature in actual operation, and the higher the temperature is, the lower the viscosity of the mixture is, and the lower the rotation speed at the moment can be.
In the above method, preferably, the graphene is prepared by a ball milling method, and is in a powder form; more preferably, when the ball milling method is adopted, the ball milling time is controlled to be 48-96 h.
According to the invention, researches show that the defects and the crystallinity of the graphene have important influence on the absorption effect of the final wave-absorbing material, the defects and the crystallinity of the graphene are few, electromagnetic waves are difficult to absorb well, the ball milling time is less than 48h, the prepared graphene product has few defects and high crystallinity, and the desired technical effect cannot be obtained.
In the above method, preferably, the ball milling method is prepared as follows:
and placing the graphite raw material and metal balls for ball milling in a ball milling tank for ball milling for 48-96h to obtain graphene powder.
In the above method, preferably, the graphite raw material includes flake graphite and/or expanded graphite.
In the above method, preferably, the apparatus used for the hot pressing and the cold pressing is a press vulcanizer.
In one embodiment, the method comprises the steps of:
placing the graphite raw material and metal balls for ball milling in a ball milling tank for ball milling for 48-96h to obtain graphene powder; wherein the graphite raw material comprises crystalline flake graphite and/or expanded graphite;
adding graphene, hollow carbon nano particles and polypropylene into a torque rheometer according to the mass ratio of 1:4:19, and banburying for 10-20min at 190 ℃ under the condition of 30-50r/min to obtain a mixture;
and hot-pressing the mixture at the temperature of 190 ℃ and 220 ℃ for 5-10min under the pressure of 15-20MPa, and then cold-pressing the mixture at the room temperature for 5min under the pressure of 20-25MPa to obtain the wave-absorbing material.
The invention also provides the wave-absorbing material prepared by the method, and the wave-absorbing material is a compound of graphene, hollow carbon nano-particles and polypropylene.
The invention has the beneficial effects that:
1) the hollow carbon nano-particles prepared by the technical scheme provided by the invention have uniform particle size and obvious hollow appearance, and can be used as a wave-absorbing medium to reduce the quality of the compound on one hand, and on the other hand, the unique hollow structure can enable incident electromagnetic waves to form multiple reflections in the cavity, so that the wave-absorbing performance of the compound is greatly improved on the basis of graphene;
2) according to the technical scheme provided by the invention, the graphene powder is prepared by adopting a ball milling method, and better graphene powder (more defects and low crystallinity) is obtained by controlling the ball milling time, so that the absorption effect on electromagnetic waves is improved; in addition, the ball milling method can realize the industrial mass production of the graphene powder;
3) the wave-absorbing material prepared by the technical scheme provided by the invention not only can effectively absorb electromagnetic waves, but also integrates the advantages of small density, fatigue resistance, chemical corrosion resistance, stress cracking resistance, easiness in forming and processing and the like of a polypropylene material; in addition, the utilization added value of the polypropylene product is greatly improved;
4) the technical scheme provided by the invention can prepare the wave-absorbing material with any size by controlling the size of the mould.
Drawings
Fig. 1 is a transmission electron micrograph of a hollow carbon nanoparticle provided in example 1;
FIG. 2 is a TEM image of the graphene powder in example 2;
fig. 3 is a raman spectrum of the graphene powder in example 2;
FIG. 4 is a reflection loss diagram of the wave-absorbing material in example 2 at 2-18 GHz;
FIG. 5 is a reflection loss chart of the wave-absorbing material in comparative example 1 at 2-18 GHz.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
The embodiment provides a preparation method of hollow carbon nanoparticles, which comprises the following steps:
adding 0.76mL of aniline, 0.58mL of pyrrole and 0.06g of non-ionic surfactant Triton X-100 into 120mL of deionized water, stirring for 0.5h, performing ultrasonic treatment for 0.5h, and then performing ice bath for 0.5h to form a clear and transparent solution (the solution is marked as a first solution); wherein the temperature of the ice bath is 0 ℃.
Dissolving 3.8g of ammonium persulfate in 30mL of deionized water to prepare an ammonium persulfate solution, and carrying out ice bath for 0.5h (the temperature of the ice bath is 0 ℃); then, the solution was added to the first solution at a time, and when the solution was added, the solution was added while stirring for about 30 seconds, to obtain a second solution.
And (3) reacting the second solution at 0 ℃ for 12 hours, washing the reacted solution by using an ethanol solution (ethanol: water is 1:3 in volume ratio) by using a vacuum filtration device after the reaction is finished until the filtrate is colorless and transparent, collecting a filter cake, and freeze-drying the collected filter cake for 48 hours to obtain a powder sample.
And (3) putting the obtained powder sample into a horizontal tubular heating furnace for carbonization treatment, wherein the carbonization temperature is 800 ℃, the temperature rise rate is 3 ℃/min, and the carbonization atmosphere is nitrogen or argon, so that the hollow carbon nano-particle powder sample is finally obtained.
A transmission electron micrograph of the hollow carbon nanoparticles provided in this example is shown in fig. 1. As can be seen from the figure: the hollow carbon nanoparticles provided by the embodiment are substantially spherical, uniform in particle size and obvious in hollow appearance.
Example 2
The embodiment provides a wave-absorbing material, which is prepared by the following steps:
preparation of graphene powder
And under the conditions of room temperature and normal pressure, 100g of crystalline flake graphite and metal balls for ball milling are placed in a ball milling tank, and ball milling is carried out for 96 hours to obtain a sample with graphite flakes peeled into graphene powder. The TEM image of the graphene powder is shown in fig. 2, in which the number of layers is small, about 8 layers. The Raman spectrogram of the graphene powder is shown in FIG. 3, and an obvious D peak can be seen, which indicates that the graphene product has more defects.
Preparation of wave-absorbing material
Adding the prepared graphene powder, the hollow carbon nanoparticles provided in the embodiment 1 and polypropylene into a torque rheometer according to the mass ratio of 1:4:19, and banburying at 190 ℃ for 20min at 50r/min to obtain a mixture;
and (3) hot-pressing the mixture on a flat vulcanizing machine for 10min under the conditions of 190 ℃ and 20MPa, and then cold-pressing for 5min under the conditions of room temperature and 25MPa to obtain the wave-absorbing material. The size of the wave-absorbing material can reach 10cm x 2mm, and the size of the wave-absorbing material can be controlled by adjusting the size of the die in the specific implementation process.
The reflection loss of the wave-absorbing material provided by the embodiment at 2-18GHz is shown in FIG. 4.
Example 3
The embodiment provides a wave-absorbing material, which is prepared by the following steps:
preparation of graphene powder
And (3) under the conditions of room temperature and normal pressure, putting 10g of crystalline flake graphite and metal balls for ball milling into a ball milling tank, and carrying out ball milling for 48 hours to obtain a sample with graphite flakes peeled into graphene powder.
Preparation of wave-absorbing material
Adding the prepared graphene powder, the hollow carbon nanoparticles provided in the embodiment 1 and polypropylene into a torque rheometer according to a mass ratio of 1:4:19, and banburying at 220 ℃ and 30r/min for 10min (the banburying speed and time are in an inverse correlation with temperature; the higher the temperature is, the smaller the viscosity of the mixture is, the smaller the required speed and time are), so as to obtain a mixture;
and (3) hot-pressing the mixture on a flat vulcanizing machine for 8min under the conditions of 190 ℃ and 15MPa, and then cold-pressing for 5min under the conditions of room temperature and 20MPa to obtain the wave-absorbing material.
Comparative example 1
The comparative example provides a wave-absorbing material, and the preparation process of the wave-absorbing material is as follows:
preparing graphene powder, wherein the preparation process is the same as that of example 2;
preparation of wave-absorbing material
Adding the prepared graphene powder and polypropylene into a torque rheometer according to the mass ratio of 1:9, and banburying for 20min at 190 ℃ at 50r/min to obtain a mixture;
and (3) hot-pressing the mixture on a flat vulcanizing machine for 10min under the conditions of 190 ℃ and 20MPa, and then cold-pressing for 5min under the conditions of room temperature and 25MPa to obtain the wave-absorbing material, wherein the wave-absorbing material is a graphene/polypropylene compound. The size of the wave-absorbing material can reach 10cm x 2mm, and the size of the wave-absorbing material can be controlled by adjusting the size of the die in the specific implementation process.
The reflection loss of the wave-absorbing material provided by the embodiment at 2-18GHz is shown in FIG. 5.
Comparative example 2
The comparative example provides a wave-absorbing material, and the preparation process of the wave-absorbing material is as follows:
preparing graphene powder in the same process as example 3;
preparation of wave-absorbing material
Adding the prepared graphene powder and polypropylene into a torque rheometer according to the mass ratio of 1:19, and banburying for 10min at 220 ℃ and 30r/min (the banburying rotation speed and time are in an inverse correlation with the temperature, the higher the temperature is, the smaller the viscosity of the mixture is, the smaller the rotation speed and time are, so as to obtain a mixture;
and (3) hot-pressing the mixture on a flat vulcanizing machine for 8min under the conditions of 190 ℃ and 15MPa, and then cold-pressing for 5min under the conditions of room temperature and 20MPa to obtain the wave-absorbing material, wherein the wave-absorbing material is a graphene/polypropylene compound.
From the reflection loss graph (figure 4) of the wave-absorbing material provided in example 2 at 2-18GHz and the reflection loss graph (figure 5) of the wave-absorbing material provided in comparative example 1 at 2-18GHz, it can be seen that: example 2 the maximum absorption peak after adding the hollow carbon nanoparticles can be increased from around-20 dB to around-50 dB for the polypropylene/graphene composite.
Claims (12)
1. A preparation method of a wave-absorbing material comprises the following steps:
adding graphene, hollow carbon nano particles and polypropylene into a torque rheometer, and banburying at 190-220 ℃ for 10-20min to obtain a mixture; the mass ratio of the graphene to the hollow carbon nanoparticles to the polypropylene is 1 (4-6) to 19; in the banburying process, the rotating speed of the torque rheometer is 30-50 r/min;
hot-pressing the mixture at the temperature of 190 ℃ and 220 ℃ for 5-10min under the pressure of 15-20MPa, and then cold-pressing the mixture at the room temperature and the pressure of 20-25MPa for 5-8min to obtain the wave-absorbing material;
the graphene is prepared by a ball milling method, and the ball milling time is controlled to be 48-96 h;
wherein, the preparation method of the hollow carbon nano-particles comprises the following steps:
mixing aniline, pyrrole, a nonionic surfactant and water to obtain a first solution;
adding an ammonium persulfate solution into the first solution after ice bath to obtain a second solution;
reacting the second solution at 0-5 ℃ for 8-16h, and then performing suction filtration, washing and freeze drying to obtain a primary product;
and carbonizing the primary product to obtain the hollow carbon nano-particles, wherein the hollow carbon nano-particles have a hollow structure which can enable incident electromagnetic waves to form multiple reflections in the cavity.
2. The method of claim 1, wherein the ratio of aniline, pyrrole, non-ionic surfactant and water is 0.76mL:0.58mL (0.04-0.16) g:120 mL.
3. The method of claim 2, wherein the non-ionic surfactant is triton X-100.
4. The method of claim 2, wherein when mixing aniline, pyrrole, non-ionic surfactant, and water, the water is deionized water.
5. The method of claim 1, wherein the method of preparing the hollow carbon nanoparticles further comprises the step of stirring, sonicating, and ice-bathing the first solution.
6. The method of claim 5, wherein the first solution is subjected to an ice bath at a temperature of 0-5 ℃ for a period of 30-50 min.
7. The method of claim 1, wherein the ammonium persulfate solution is obtained by dissolving ammonium persulfate in deionized water.
8. The method of claim 7, wherein the ratio of ammonium persulfate to deionized water is 3.8g:30 mL.
9. The method of claim 1, wherein when the ammonium persulfate solution is subjected to the ice bath, the temperature of the ice bath is 0-5 ℃, and the time of the ice bath is 30-50 min.
10. The method as claimed in claim 1, wherein the temperature of the carbonization treatment is 700-900 ℃.
11. The method according to claim 10, wherein the atmosphere of the carbonization treatment is nitrogen or argon.
12. A wave-absorbing material obtainable by a process according to any one of claims 1 to 11.
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| CN108448101B (en) * | 2018-04-12 | 2020-06-19 | 深圳大学 | Lithium-sulfur battery positive electrode material and preparation method and application thereof |
| CN108439369B (en) * | 2018-04-12 | 2020-06-19 | 深圳大学 | Nitrogen-oxygen co-doped hollow carbon nano-microsphere as well as preparation method and application thereof |
| CN108865061A (en) * | 2018-07-14 | 2018-11-23 | 合肥艾飞新材料有限公司 | A kind of hollow plumbago alkene microballoon and preparation method thereof |
| CN109879635A (en) * | 2019-04-15 | 2019-06-14 | 苏州安洁新材料有限公司 | A kind of ultra-thin high magnetic permeability inhales wave plate and its casting slurry and preparation method |
| CN110060834B (en) * | 2019-05-16 | 2021-06-08 | 常州威斯双联科技有限公司 | Soft magnetic alloy powder, wave absorbing plate, preparation method of soft magnetic alloy powder, electronic component and electronic equipment |
| CN110041886A (en) * | 2019-05-21 | 2019-07-23 | 常州威斯双联科技有限公司 | A kind of novel graphene absorbing material and preparation method |
| CN110487866B (en) * | 2019-09-19 | 2022-01-28 | 西北师范大学 | Preparation and application of porous hollow carbon nanosphere material |
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