CN114958301B - Carbon nano tube/Ni porphyrin loaded wave-absorbing material, preparation method and application thereof - Google Patents
Carbon nano tube/Ni porphyrin loaded wave-absorbing material, preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of wave-absorbing materials, and particularly relates to a carbon nano tube/Ni porphyrin loaded wave-absorbing material, and a preparation method and application thereof. The carbon nano tube/Ni porphyrin loaded wave absorbing material is of a one-dimensional tubular interwoven three-dimensional network structure, and the fiber consists of a CNTs matrix and a Ni-TAPP loaded thin layer, wherein the Ni-TAPP loaded thin layer is distributed on the surface of the CNTs matrix. The method comprises the following steps: (1) Mixing Ni-TAPP and DMF solution, CNTs and DMF solution and standing; (2) And (3) centrifugally cleaning, collecting and drying the reactant after standing. According to the invention, ni-TAPP and CNTs are effectively subjected to nanoscale compounding, and the prepared material has excellent performance.
Description
Technical Field
The invention belongs to the field of wave-absorbing materials, and particularly relates to a carbon nano tube/Ni porphyrin loaded wave absorber, and a preparation method and application thereof.
Background
The information disclosed in the background of the invention is only for enhancement of understanding of the general background of the invention and is not necessarily to be taken as an admission or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
In recent years, lightweight high performance Carbon Nanotubes (CNTs) have received attention because of their unique advantages over conventional metallic electromagnetic wave absorbing materials. However, an excessively high dielectric constant of the carbon nanotube results in poor impedance matching of the carbon material with air, and thus, poor electromagnetic wave absorption performance thereof. To overcome this obstacle, the general idea is to load magnetic particles such as Fe, co, ni, etc. However, the density of the supported particles is, without exception, much higher than CNTs, resulting in a very high density composite. In addition, the complex preparation process and easy oxidation limit the further application of the catalyst. Therefore, it remains a significant challenge to explore a light-weight, high-chemical-stability, high-efficiency carbon nanotube-based electromagnetic wave absorbing material.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a carbon nano tube/Ni porphyrin loaded wave-absorbing material, and a preparation method and application thereof. The CNTs/Ni porphyrin material is effectively compounded in nanometer scale, and the prepared CNTs/Ni porphyrin loaded composite material has the characteristics of high absorption strength, thin matching thickness, light weight, strong oxidation resistance and the like.
In order to achieve the above purpose, the present invention discloses the following technical solutions:
in a first aspect of the invention, a carbon nanotube/Ni porphyrin loaded wave-absorbing material is provided.
A carbon nano tube/Ni porphyrin loaded wave absorbing material is of a three-dimensional network structure with one-dimensional fibers interwoven with each other, wherein the one-dimensional fibers consist of a carbon nano tube matrix and a 5,10,15, 20-tetra (4-aminophenyl) porphyrin nickel loaded thin layer, and the 5,10,15, 20-tetra (4-aminophenyl) porphyrin nickel loaded thin layer is distributed on the surface of the carbon nano tube matrix.
As a further technical scheme, in the wave-absorbing material, the weight percentage of Ni in the one-dimensional fiber is 0.03% -0.23%. The loading (weight percent) of 5,10,15, 20-tetra (4-aminophenyl) porphyrin is 0.37-2.86%.
As a further technical scheme, in the wave-absorbing material, the length of the one-dimensional fiber is 10-30 mu m, and the diameter is 10-20nm.
Porphyrin and its derivatives have wide electron conjugation, stable central metal ion and structure cutting capacity, and are ideal candidates for developing wave absorbing materials. After the porphyrin is combined with CNTs, a rich heterogeneous structure can be formed at the interface, which is likely to be more beneficial to the regulation and control of the electromagnetic parameters of the CNTs. In addition, porphyrin derivatives with pi planar structures can build multidimensional heterostructures on the pi-electron plane of carbon nanotubes and produce intimate electrical contact at the interface between the two.
According to the invention, the porphyrin derivative [5,10,15, 20-tetra (4-aminophenyl) porphyrin nickel, ni-TAPP ] is effectively combined with CNTs under the drive of non-covalent pi-pi interaction through a simple self-assembly method for the first time. The minimum value of the Reflection Loss (RL) of the material is 66.5dB (10.1 GHz,1.9 mm), and the filling rate is as low as 2.86%. The remarkable improvement of the performance is derived from the cooperation of the structure and the function, so that the optimized impedance matching, reasonable conduction loss and enhanced interface polarization are ensured.
The invention is characterized in that the wave-absorbing material is prepared by the following steps: the superior performance of Ni-TAPP@CNTs compared to CNTs is due to the synergistic effect of Ni-TAPP and CNTs. First, CNTs with good conductivity provide a long channel for the continuous flow of electrons, which may increase conduction losses. In addition, CNTs can be easily built into three-dimensional conductive networks, which further increases conduction losses and provides a pathway for the diffusion of accumulated energy. Secondly, after the Ni-TAPP is introduced to the surface of the carbon nano tube, the porphyrin has good semiconductor performance, and the Ni-TAPP@CNTs composite material can obtain proper conductivity, so that the advantages of the carbon nano tube and the Ni-TAPP are utilized, good impedance matching is realized, and the conductivity loss is optimized. The introduction of Ni-TAPP results in the occurrence of magnetic losses including natural resonance or exchange resonance, which further results in damping capacity. Third, porphyrin molecules provide single-atom metal centers that are completely dispersed and orderly distributed, thereby effectively reducing metal loading. In addition, the Ni-TAPP@CNTs nano tube with a special hollow structure and a three-dimensional network can improve dielectric loss and promote multiple reflection and absorption.
The invention provides a preparation method of a carbon nano tube/Ni porphyrin loaded wave-absorbing material, which comprises the following steps:
dispersing the carbon nano tube in DMF solution, and then soaking the dispersed carbon nano tube in Ni-TAPP DMF solution for 24 hours; centrifuging, cleaning and drying to obtain the carbon nanotube/Ni porphyrin loaded wave-absorbing material.
As a further technical scheme, centrifuging the reaction mixture at 10000rpm for 10min, washing with DMF for 3-5 times to remove excessive Ni-TAPP, and drying to obtain Ni-TAPP loaded CNTs.
As a further technical scheme, the different Ni-TAPP loadings in Ni-TAPP@CNTs are controlled by controlling the concentration of the solution of Ni-TAPP added in DMF, and the concentration can be 0.1-10mg/mL, and further, 1-2mg/mL.
As a further technical scheme, the carbon nano tube is dispersed in DMF solution, and the concentration of the carbon nano tube in DMF solution is 0.1-1.2mg/mL.
As a further technical scheme, the condition that the carbon nano tube is dispersed in DMF is that 20mg of the carbon nano tube is dispersed in 4mL of DMF solution, and the ultrasonic action is carried out for 3h.
As a further technical scheme, the reaction mixture is centrifuged at 10000rpm for 10min.
As a further technical scheme, the carbon nanotube drying condition is that the carbon nanotube is dried in vacuum for 12 hours at 90 ℃.
The principle of the preparation method is pi-pi interaction driven in-situ self-assembly.
The invention utilizes a self-assembly method to prepare the hollow carbon nanotube-loaded composite material, and constructs a mutually-interweaved reticular structure, so that the microstructure can provide larger specific surface area and long-range conductivity loss, is beneficial to multiple reflection and multiple scattering of electromagnetic waves and is beneficial to further improvement of electromagnetic wave absorption performance; meanwhile, the interwoven net structure can effectively introduce air, reduce the relative dielectric constant of the material and is beneficial to improving the impedance matching performance of the material.
In a third aspect of the present invention, there is provided a carbon nanotube/Ni porphyrin-loaded electromagnetic wave absorber, which is formed by compounding paraffin and a carbon nanotube/Ni porphyrin-loaded wave absorbing material prepared according to the present invention. Preferably, 90wt% of paraffin wax and 10wt% of a carbon nanotube/Ni porphyrin loaded wave-absorbing material.
In a fourth aspect, the present invention provides applications of the carbon nanotube/Ni porphyrin-loaded wave absorbing material and the carbon nanotube/Ni porphyrin-loaded electromagnetic wave absorber in radio communication systems, high-frequency prevention, microwave heating equipment, construction of microwave darkroom, stealth technology, and the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) The Ni-TAPP@CNTs wave-absorbing material prepared by the method has multiple loss characteristics, has excellent impedance matching performance and unique microscopic morphology, can keep proper dielectric constant in a high-frequency range, and has very excellent electromagnetic wave absorption performance.
(2) The carbon nano tube has the characteristic of light weight, and the supported porphyrin material has low density and small load capacity, so the Ni-TAPP@CNTs wave absorbing material prepared by the invention can be used for preparing a light electromagnetic wave absorber with thin thickness.
(3) The Ni-TAPP@CNTs wave-absorbing material prepared by the method has excellent impedance matching performance; the effective absorption frequency bandwidth of the manufactured absorber can reach 6.8GHz under the condition of single matching thickness.
(4) The Ni-TAPP@CNTs wave-absorbing material prepared by the method has uniform scale and strong oxidation resistance and corrosion resistance.
(5) The preparation process is simple, and complex hardware equipment is not needed. Meanwhile, the manufacturing cost is low, and the method is very suitable for industrial production.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is an SEM image of Ni-TAPP@CNTs wave-absorbing material prepared in example 1 of the present invention.
FIG. 2 is a TEM image of Ni-TAPP@CNTs wave-absorbing material prepared in example 1 of the present invention.
FIG. 3 is an XRD diffraction pattern of Ni-TAPP@CNTs wave-absorbing material prepared in example 1 of the present invention.
FIG. 4 shows the electromagnetic wave absorption curve of Ni-TAPP@CNTs wave absorbing material prepared in example 1 of the present invention.
FIG. 5 is an electromagnetic wave absorption curve of Ni-TAPP@CNTs wave absorbing material prepared in test example 1 of the present invention.
FIG. 6 is an electromagnetic wave absorption curve of the unloaded CNTs wave absorbing material prepared in test example 2 of the present invention.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present invention. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
As described above, the CNTs as a conductive loss type carbonaceous wave-absorbing material cannot provide proper dielectric polarization loss and magnetic loss, and thus loss performance is not high enough. It is known from the impedance matching condition in the theory of electromagnetic wave absorption that if the impedance matching condition is satisfied only by a single carbon material, it is difficult to obtain excellent electromagnetic wave absorption performance, which limits its further development and application. Therefore, the invention provides a Ni-TAPP@CNTs wave-absorbing material and a preparation method thereof; the invention will now be further described with reference to the drawings and detailed description.
Example 1
A preparation method of Ni-TAPP@CNTs wave-absorbing material comprises the following steps:
20mg of CNTs were dispersed in 4mL of DMF solution, sonicated for 3h, and then the dispersed CNTs were immersed in 2mg/mL of Ni-TAPP in DMF for 24h. Centrifuging the reaction mixture at 10000rpm for 10min, washing with DMF for 3-5 times to remove excessive Ni-TAPP, and vacuum drying at 90 ℃ for 12h to obtain Ni-TAPP@CNTs-2.
Example 2
A preparation method of Ni-TAPP@CNTs wave-absorbing material comprises the following steps:
20mg of CNTs were dispersed in 4mL of DMF solution, sonicated for 3h, and then the dispersed CNTs were immersed in 1mg/mL of Ni-TAPP in DMF for 24h. Centrifuging the reaction mixture at 10000rpm for 10min, washing with DMF for 3-5 times to remove excessive Ni-TAPP, and vacuum drying at 90 ℃ for 12h to obtain Ni-TAPP@CNTs-1.
Test example 1
A preparation method of a no-load CNTs wave-absorbing material comprises the following steps:
CNTs are reagent grade, available from XFNNO Inc/Co. (10-30 μm length, 10-20nm diameter) for use with the materials received.
Performance test:
(1) The results of observation of the Ni-TAPP@CNTs wave-absorbing material prepared in example 1 under SEM and TEM are shown in FIG. 1 and FIG. 2, respectively, and can be seen: after Ni-TAPP is loaded, ni-TAPP@CNTs are still in a tubular form, and the surface of MWCNTs of the Ni-TAPP@CNTs-2 hybrid material is uniformly coated with a growing Ni-TAPP thin layer nano shell. In addition, no diffraction rings were found in the TEM image, indicating that Ni-TAPP@CNTs were completely free of crystallinity.
(2) XRD testing was conducted on the Ni-TAPP@CNTs wave-absorbing material prepared in example 1, and the results are shown in FIG. 3, and it can be seen that: all of the pristine carbon nanotubes Ni-TAPP@CNTs-1 and Ni-TAPP@CNTs-2 have a common characteristic peak at 2 theta value of about 25.8 DEG, which is a hexagonal graphite characteristic diffraction peak of the carbon nanotube (002) plane. Ni-TAPP@CNTs-1 and Ni-TAPP@CNTs-2 have a broad peak at 2θ=21.29°, which is due to the pi-pi stacking distance between the porphyrin ring and the carbon nanotubes. Furthermore, the XRD pattern of Ni-tapp@cnts-2 shows a relatively weak peak at 2θ=19.16°, which is refracted from the (300) plane of TAPP, indicating a long-range order distribution of the molecule along that direction.
(3) Inductively coupled plasma emission spectrometry (ICP) test was performed on the Ni-TAPP@CNTs wave-absorbing material prepared in example 1, and the Ni mass ratios (wt.%) of Ni-TAPP@CNTs-1 and Ni-TAPP@CNTs-2 were 0.03% and 0.23%, respectively, from which the load mass ratios of porphyrins were calculated to be 0.37% and 2.86%, respectively.
(4)The Ni-TAPP@CNTs-2 absorbing material prepared in example 1 was mixed with paraffin wax in a mass ratio of 1:9 and then pressed into a ring-shaped absorber sample (D Outer part ×d Inner part The relevant parameters are measured by using a Agilent Technologies E8363A electromagnetic wave vector network analyzer, the electromagnetic wave absorption curve of the absorber is shown in figure 4, the matching thickness is 1.9mm, the maximum absorption intensity is achieved at the frequency of 10.1GHz, the reflection loss is-66.5 dB, and the sample has extremely strong electromagnetic wave loss capacity.
(5) The Ni-TAPP@CNTs-1 absorbing material prepared in example 2 was mixed with paraffin wax in a mass ratio of 1:9 and then pressed into a ring-shaped absorber sample (D Outer part ×d Inner part X h=7×3.04×2.0 mm), the relevant parameter ε r Sum mu r As measured by using a Agilent Technologies E8363A electromagnetic wave vector network analyzer, the electromagnetic wave absorption curve of the absorber is shown in fig. 5, and it can be seen that the material maintains a certain absorption strength due to the reduction of the Ni-TAPP deficiency load, but the matching resistance of the material is poor, the matching thickness is obviously improved, and the application of the material in the aspect of electromagnetic wave absorption is limited, but the absorption band under a larger thickness is widened, so that the material can be applied to a small number of special fields.
(6) The unloaded MWCNTs wave-absorbing material prepared in test example 1 was mixed with paraffin wax in a mass ratio of 1:9, and then pressed into a ring-shaped absorber sample (D Outer part ×d Inner part X h=7×3.04×2.0 mm), the relevant parameter ε r Sum mu r As shown in FIG. 6, the electromagnetic wave absorption curve of the absorber is measured by using a Agilent Technologies E8363A electromagnetic wave vector network analyzer, the absorption strength of the material is greatly reduced due to the lack of the load of Ni-TAPP, but the matching resistance of the material is further deteriorated, the matching thickness is further improved, the electromagnetic wave absorption is not facilitated, and the application of the material in the aspect of electromagnetic wave absorption is greatly limited.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The preparation method of the CNTs/Ni porphyrin loaded wave-absorbing material is characterized by comprising the following steps of:
dispersing carbon nanotubes in DMF solution, and then soaking the dispersed carbon nanotubes in DMF solution of 5,10,15, 20-tetra (4-aminophenyl) porphyrin nickel for 24 hours; centrifuging, cleaning and drying the reaction mixture to obtain the CNTs/Ni porphyrin loaded wave-absorbing material;
the condition that the carbon nano tube is dispersed in DMF is that 20mg carbon nano tube is dispersed in 4mL DMF solution, and the ultrasonic effect is 3 h;
the concentration of the solution of the 5,10,15, 20-tetra (4-aminophenyl) porphyrin nickel in DMF is 2 mg/mL;
the CNTs/Ni porphyrin-loaded wave-absorbing material is of a three-dimensional network structure with one-dimensional fibers interwoven with each other, wherein the one-dimensional fibers consist of a carbon nanotube matrix and a 5,10,15, 20-tetra (4-aminophenyl) porphyrin nickel-loaded thin layer, and the 5,10,15, 20-tetra (4-aminophenyl) porphyrin nickel-loaded thin layer is distributed on the surface of the carbon nanotube matrix;
in the one-dimensional fiber, the weight percentage of Ni is 0.03%; the weight percentage of 5,10,15, 20-tetra (4-aminophenyl) porphyrin was 0.37%.
2. The method according to claim 1, wherein the one-dimensional fiber has a length of 10 to 30 μm and a diameter of 10 to 20nm.
3. The method of claim 1, wherein the centrifugation conditions are: centrifuging at 10000rpm for 10 min; and the cleaning is to use DMF for 3-5 times.
4. The method of claim 1, wherein the carbon nanotube drying condition is vacuum drying 12h at 90 ℃.
5. The carbon nano tube/Ni porphyrin loaded electromagnetic wave absorber is characterized by being formed by compounding paraffin and the CNTs/Ni porphyrin loaded electromagnetic wave absorbing material prepared by the preparation method of any one of claims 1-4.
6. The CNTs/Ni porphyrin-loaded wave-absorbing material prepared by the preparation method of any one of claims 1-4 and/or the carbon nano tube/Ni porphyrin-loaded electromagnetic wave absorber of claim 5 are applied to a radio communication system, a high-frequency-resistant microwave heating device, a microwave darkroom construction and a stealth technology.
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