CN111454691A - Graphene/amorphous titanium dioxide nanorod composite material, preparation method and application thereof - Google Patents
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Abstract
A graphene/amorphous titanium dioxide nanorod composite material, a preparation method and application thereof belong to the field of electromagnetic wave absorption. The composite material takes graphene oxide and tetrabutyl titanate as raw materials, the graphene oxide is reduced into graphene by a one-step hydrothermal method, and simultaneously, titanium elements in the tetrabutyl titanate uniformly grow on two surfaces of a graphene sheet layer in the form of amorphous titanium dioxide nanorods under the action of a hydrothermal process, and finally the graphene/amorphous titanium dioxide nanorod composite material is formed. Wherein, the length and the width of the graphene sheet layer in the obtained composite material are both between 1 and 8 mu m, and the length of the amorphous titanium dioxide nano rod is about 300 to 500 nm. The composite material prepared by the invention can effectively absorb electromagnetic waves, and the absorption frequency band can cover Ku wave band (2-2.5mm), X wave band (2.5-3.5mm) and most of C wave band (3.5-5.5mm) of radar wave band by adjusting the thickness of the composite material.
Description
Technical Field
The invention belongs to the field of electromagnetic wave absorption, relates to a graphene/amorphous titanium dioxide nanorod composite material, a preparation method and application thereof, and particularly relates to a nanocomposite material, a synthesis method thereof and electromagnetic wave absorption performance of the nanocomposite material.
Background
In recent times, due to the rapid development of high and new technologies and the improvement of living standards of people, various electronic and electrical devices bring great convenience to the life of people, and meanwhile, the radiation of electromagnetic energy from various electronic devices may affect the health of people. In addition, in military applications, excessive electromagnetic radiation or reflections can easily cause own military equipment to be detected by enemy radar and thus hit. Therefore, it is required to develop an efficient electromagnetic wave absorbing material in both life and military.
Firstly, the high-efficiency wave-absorbing performance and the simple synthesis method are not compatible, if the composite material with the excellent wave-absorbing performance is desired to be obtained, a plurality of materials are required to be compounded to increase a loss mechanism, which inevitably leads to the increase of the synthesis difficulty [ L iu, Panbo, Huang, Ying, Yan, J, ACS applied materials ], the absorption performance of the material is reduced due to the fact that the conductivity of the carbon material is too high, and the reflection of the material surface to electromagnetic waves is increased, and the electromagnetic waves often cannot effectively enter the material, so that the absorption performance of the material is reduced&interfaces,2016,8(8):5536-5546.][Yin,Xiaowei,Hou,Zexin,Zhang,Litong,et al.Carbon:An InternationalJournal Sponsored by the American Carbon Society,2017,116:50-58.]. Secondly, most of the existing work adopts a composite magnetic nanoparticle mode to adjust the electromagnetic parameters of the carbon material and TiO2In contrast, the magnetic material has a relatively high density and is not sufficiently stable [ Ya L i, Xiaoofang L iu, Xiaoyu Nie, et al advanced functional Materials,2019,29(10): n ^ na-n/a.]And the application of the wave-absorbing material is limited to a certain extent.
The graphene has a unique two-dimensional structure, a large specific surface area, extremely high electric conductivity, thermal conductivity and electron mobility, is suitable for being used as a light wave-absorbing material, has better dispersibility in a solution compared with other carbon materials such as carbon nanotubes and the like, and is favorable for synthesizing a more uniform composite material. If the graphene is mixed with TiO2The composite material has larger effective absorption bandwidth due to the difference of the two materials in the dimension, and the lightweight wave-absorbing material is easy to form due to the smaller density of the two materials, and the TiO material is easy to form2The nano-rod and the graphene are compounded, so that more contact sites can be provided to increase the effect of interface loss, and the wave absorbing performance of the composite material is improved.
At present, various methods have been reported for synthesizing titanium dioxide/graphene composite materials, for example, titanium dioxide is directly used as a precursor to be synthesized in situ on the surface of graphene [ Zhang, y.; zhang, n.; tang, z.r.; xu, Y.J. physicalchemistry chemical physics: PCCP 2012,14,9167.]Preparing TiO by adopting electrochemical method to synchronously reduce graphene in situ and carrying out anodic oxidation2[Pan,X.；Zhao,Y.；Liu,S.；Korzeniewski,C.L.；Wang,S.；Fan,Z.Y.Acs Applied Materials&Interfaces 2012,4,3944.]Respectively in graphene and TiO2After the surface modification of the organic functional groups, the two are formed into a composite material by an esterification reaction [ Zhang, K.; Kemp, K.C.; Chandra, V.Mater L ett 2012,81,127 ].]However, the reported synthetic method is too complicated, and is not favorable for mass synthesis and application of the composite material. On the other hand, consider amorphous TiO2Compared with a crystalline state, the composite material has more defects and oxygen vacancies, the defects can be used as sites for dipole polarization to enhance the electromagnetic loss mechanism of the material, and the existing reports do not show that the graphene/amorphous titanium dioxide composite material is used for the research of the wave-absorbing field, so that the synthesis and wave-absorbing characteristic research of the graphene/amorphous titanium dioxide composite material has uniqueness and innovation. In short, it is necessary to reasonably construct the microstructure of the composite material, take account of the interface contact site and the conductivity, and simplify the synthesis process under the premise of ensuring the wave absorption performanceThe method achieves the aims of simple preparation and high-efficiency wave absorption of the titanium dioxide/graphene composite material.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a graphene/amorphous titanium dioxide nanorod composite material, a preparation method and application thereof in electromagnetic wave absorption.
In order to achieve the purpose, the invention adopts the technical scheme that:
a graphene/amorphous titanium dioxide nanorod composite material is prepared by using graphene oxide and tetrabutyl titanate as raw materials, reducing graphene oxide into graphene through a one-step hydrothermal method, and enabling titanium elements in tetrabutyl titanate to uniformly grow on two surfaces of a graphene sheet layer in the form of amorphous titanium dioxide nanorods under the action of a hydrothermal process, so that the graphene/amorphous titanium dioxide nanorod composite material is finally formed (shown in figures 1-4). Wherein the length and the width of the graphene sheet layer in the obtained composite material are both 1-8 mu m, and the length of the amorphous titanium dioxide nanorod is 300-500 nm.
The graphene/amorphous titanium dioxide nanorod composite material prepared by the invention has the advantages that the surface of amorphous titanium dioxide contains a large number of oxygen-containing groups, and compared with other types of titanium oxide, the amorphous titanium dioxide nanorod composite material is easier to link with the oxygen-containing groups on the surface of graphene to form a stable composite material, and in addition, the oxygen-containing groups can also be used as dipole polarization sites to enhance the wave absorbing performance. The invention is a high-efficiency wave-absorbing material with excellent performance, on one hand, the difference of the two materials in the dimension can lead the composite material to have larger effective absorption bandwidth, and the light wave-absorbing material is easy to form because the densities of the two materials are smaller; on the other hand, amorphous TiO2Compared with other TiO2More defects and oxygen vacancies are used as dipole polarization sites, so that the electromagnetic loss is enhanced; in addition, the nano rod-shaped structure can provide more contact sites to maximize the effect of interface loss, and the wave absorbing performance of the composite material is improved.
A preparation method of a graphene/amorphous titanium dioxide nanorod composite material is characterized in that graphene oxide and tetrabutyl titanate are converted into the graphene/amorphous titanium dioxide nanorod composite material through a one-step hydrothermal method, wherein amorphous titanium dioxide nanorods are uniformly dispersed on a graphene sheet layer. The method comprises the following steps:
uniformly dispersing graphene oxide in absolute ethyl alcohol serving as a solvent, performing ultrasonic treatment to uniformly disperse the graphene oxide, and then sequentially dropwise adding glycerol and tetrabutyl titanate, wherein the glycerol is used as a morphology control agent, and after the ultrasonic treatment, placing the mixed solution in a reaction kettle to perform hydrothermal reaction at the reaction temperature of 180 ℃ for 15 hours; and carrying out alcohol suction filtration and freeze-drying to obtain the graphene/amorphous titanium dioxide nanorod composite material. By changing the addition ratio of the graphene oxide to the tetrabutyl titanate, graphene/amorphous titanium dioxide nanorod composite materials with different composite densities can be obtained, so that the electromagnetic parameters of the composite materials are comprehensively adjusted, and the composite materials have high-efficiency electromagnetic wave absorption performance.
The mass ratio of the titanium element in the graphene oxide to the tetrabutyl titanate is (0.1-10): 1, preferably (1-2): 1, and more preferably 1: 1. When the graphene oxide is excessive, the conductivity is too high, the reflection of electromagnetic waves is increased, and the wave-absorbing property is weakened; when the titanium dioxide is excessive, the conductivity is too weak, the dielectric loss is reduced, and the wave-absorbing property is also reduced.
75mg of graphene oxide powder and 5ml of glycerol are correspondingly added into each 25ml of absolute ethyl alcohol.
In the suction filtration process, the filter membrane is a polytetrafluoroethylene microporous filter membrane.
The first ultrasonic time is 2 hours, and the second ultrasonic time is 20 min.
According to the invention, absolute ethyl alcohol is used as a solvent in the hydrothermal process, so that the reduction degree of graphene oxide can be improved, and the conductive capability of graphene in the composite material is enhanced. The glycerol is selected as the morphology control agent, so that the successful synthesis of the nano-rod-shaped titanium dioxide can be ensured, the interfacial polarization site of the composite material is maximized, and the wave-absorbing performance is enhanced.
A graphene/amorphous titanium dioxide nanorod composite material is applied to the field of electromagnetic wave absorption and is used as a wave-absorbing and electromagnetic shielding material.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the graphene/amorphous titanium dioxide nanorod wave-absorbing material with excellent performance is successfully synthesized by only one-step hydrothermal method, the preparation process is simple and easy to implement, the requirement on experimental conditions is low, the experimental raw materials are cheap and easy to obtain, and the method is suitable for mass preparation.
(2) According to the invention, graphene with large specific surface area and high conductivity and titanium dioxide with excellent dielectric property are combined, so that on one hand, larger scale difference can be generated, the effective absorption bandwidth of the material can be increased, on the other hand, the nano rod-shaped structure can provide more contact sites to maximize the effect of interface loss, and the wave-absorbing property of the composite material is improved.
(3) From the angle of an electromagnetic loss mechanism, the invention firstly proposes that the amorphous titanium dioxide is compounded with the graphene to enhance the wave absorbing performance of the material and greatly simplify the synthesis steps of the composite material. The obtained graphene/amorphous titanium dioxide nanorod composite material not only maintains the light characteristics and the electromagnetic loss mechanism of matrix titanium dioxide and graphene, but also optimizes the impedance matching characteristic of the material, and increases new loss mechanisms such as interface polarization.
(4) The graphene/amorphous titanium dioxide nanorod composite material prepared by the invention can effectively absorb electromagnetic waves, and the absorption frequency band can cover Ku (2-2.5mm), X (2.5-3.5mm) and most of C (3.5-5.5mm) of radar wave bands by adjusting the thickness of the composite material, so that the material is simple and easy to obtain, is suitable for mass preparation, and has wide application prospects in the field of electromagnetic wave absorption (fig. 7 and 8).
Drawings
FIG. 1 is an SEM image of a graphene/amorphous titanium dioxide nanorod composite material prepared in example 4;
FIG. 2 is an SEM image of the graphene/amorphous titanium dioxide nanorod composite material prepared in example 5;
FIG. 3 is a TEM image of the graphene/amorphous titanium dioxide nanorod composite material prepared in example 1;
FIG. 4 is a TEM image of the graphene/amorphous titanium dioxide nanorod composite material prepared in example 5;
FIG. 5 is a TEM diffraction pattern of the graphene/amorphous titanium dioxide nanorod composite material prepared in example 5;
FIG. 6 is a TEM diffraction pattern of the graphene/crystalline titanium dioxide nanorod composite material prepared in example 6;
FIG. 7 is a reflection loss (wave-absorbing property) diagram of the graphene/amorphous titanium dioxide nanorod composite material prepared in example 1;
FIG. 8 is a reflection loss (wave-absorbing property) diagram of the graphene/amorphous titanium dioxide nanorod composite material prepared in example 5;
fig. 9 is a reflection loss (wave-absorbing property) diagram of the graphene/crystalline titanium dioxide nanorod composite material prepared in example 6.
Detailed Description
The present invention is further illustrated in detail below by way of examples. It is to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art in light of the foregoing description are intended to be included within the scope of the invention. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Examples 1
Firstly, dispersing 75mg of graphene oxide powder in 25ml of absolute ethyl alcohol, performing ultrasonic treatment for 2 hours to uniformly disperse the graphene oxide powder, then sequentially dropwise adding 5ml of glycerol and 0.25ml of tetrabutyl titanate, then performing ultrasonic treatment on the mixed solution for 20 minutes, pouring the obtained mixed solution into a lining of a polytetrafluoroethylene reaction kettle with the capacity of 100ml, placing the reaction kettle at 180 ℃ for reaction for 15 hours, washing the obtained product for 3 times by using an alcohol suction filtration method, selecting a polytetrafluoroethylene microporous filter membrane as the filter membrane, and finally freeze-drying the obtained powdery solid in a freeze dryer for 24 hours to obtain the graphene/amorphous titanium dioxide nanorod composite material (the mass ratio of the titanium element in the graphene oxide and the tetrabutyl titanate is 2: 1).
And carrying out field emission scanning electron microscope analysis and transmission electron microscope analysis on the obtained material, wherein the obtained results are shown in figures 1-5. It can be seen from FIGS. 1 to 4 (i.e., the scanning electron microscope image and the transmission electron microscope image of the graphene/amorphous titanium dioxide nanorod composite material) that titanium dioxide is uniformly dispersed in the form of nanorods into the microstructure of graphene, and the synthesized TiO can be obtained by referring to the TEM diffraction pattern of FIG. 52Is amorphous TiO2Therefore, the obtained product can be determined to be the target product graphene/amorphous titanium dioxide nanorod composite wave-absorbing material.
The wave absorbing performance of the composite material is tested by adopting a vector network analyzer, the obtained graphene/amorphous titanium dioxide nanorod composite material sample powder and paraffin powder are mixed according to the mass ratio of 1: 4 to prepare a standard die, the vector network analyzer is used for testing the electromagnetic parameters of a sample in the range of 2-18 GHz, and an electromagnetic wave absorbing curve is calculated and drawn according to a related formula, as shown in figure 7, it can be seen from figure 7 that the graphene-based lead composite wave absorbing material prepared in the embodiment shows good wave absorbing performance on low-frequency to high-frequency electromagnetic waves, when the thickness is 3mm, the maximum attenuation value reaches-17 dB at 11.7GHz, the width of an effective absorption band ((R L < -10dB)) reaches 4.5GHz (12.3-16.8GHz), 90% of attenuation on the microwaves can be realized, and the graphene-based lead composite wave absorbing material is expected to be practically applied to wave absorbing and electromagnetic shielding materials.
EXAMPLES example 2
Firstly, dispersing 75mg of graphene oxide powder in 25ml of absolute ethyl alcohol, performing ultrasonic treatment for 2 hours to uniformly disperse the graphene oxide powder, then sequentially dropwise adding 5ml of glycerol and 0.05ml of tetrabutyl titanate, then performing ultrasonic treatment on the mixed solution for 20 minutes, pouring the obtained mixed solution into a lining of a polytetrafluoroethylene reaction kettle with the capacity of 100ml, placing the reaction kettle at 180 ℃ for reaction for 15 hours, washing the obtained product for 3 times by using an alcohol suction filtration method, selecting a polytetrafluoroethylene microporous filter membrane as the filter membrane, and finally freeze-drying the obtained powdery solid in a freeze dryer for 24 hours to obtain the graphene/amorphous titanium dioxide nanorod composite material (the mass ratio of the titanium element in the graphene oxide and the tetrabutyl titanate is 10: 1).
EXAMPLE 3
Firstly, dispersing 75mg of graphene oxide powder in 25ml of absolute ethyl alcohol, performing ultrasonic treatment for 2 hours to uniformly disperse the graphene oxide powder, then sequentially dropwise adding 5ml of glycerol and 0.1ml of tetrabutyl titanate, then performing ultrasonic treatment on the mixed solution for 20 minutes, pouring the obtained mixed solution into a lining of a polytetrafluoroethylene reaction kettle with the capacity of 100ml, placing the reaction kettle at 180 ℃ for reaction for 15 hours, washing the obtained product for 3 times by using an alcohol suction filtration method, selecting a polytetrafluoroethylene microporous filter membrane as the filter membrane, and finally freeze-drying the obtained powdery solid in a freeze dryer for 24 hours to obtain the graphene/amorphous titanium dioxide nanorod composite material (the mass ratio of the titanium element in the graphene oxide and the tetrabutyl titanate is 5: 1).
EXAMPLE 4
Firstly, dispersing 75mg of graphene oxide powder in 25ml of absolute ethyl alcohol, performing ultrasonic treatment for 2 hours to uniformly disperse the graphene oxide powder, then sequentially dropwise adding 5ml of glycerol and 5ml of tetrabutyl titanate, then performing ultrasonic treatment on the mixed solution for 20 minutes, pouring the obtained mixed solution into a lining of a polytetrafluoroethylene reaction kettle with the capacity of 100ml, placing the reaction kettle at 180 ℃ for reaction for 15 hours, washing the obtained product for 3 times by using an alcohol suction filtration method, selecting a polytetrafluoroethylene microporous filter membrane as the filter membrane, and finally freeze-drying the obtained powdery solid in a freeze dryer for 24 hours to obtain the graphene/amorphous titanium dioxide nanorod composite material (the mass ratio of titanium elements in the graphene oxide and the tetrabutyl titanate is 0.1: 1).
EXAMPLE 5
Firstly, dispersing 75mg of graphene oxide powder in 25ml of absolute ethyl alcohol, performing ultrasonic treatment for 2 hours to uniformly disperse the graphene oxide powder, then sequentially dropwise adding 5ml of glycerol and 0.5ml of tetrabutyl titanate, then performing ultrasonic treatment on the mixed solution for 20 minutes, pouring the obtained mixed solution into a lining of a polytetrafluoroethylene reaction kettle with the capacity of 100ml, placing the reaction kettle at 180 ℃ for reaction for 15 hours, washing the obtained product for 3 times by using an alcohol suction filtration method, selecting a polytetrafluoroethylene microporous filter membrane as the filter membrane, and finally freeze-drying the obtained powdery solid in a freeze dryer for 24 hours to obtain the graphene/amorphous titanium dioxide nanorod composite material (the mass ratio of the titanium element in the graphene oxide and the tetrabutyl titanate is 1: 1).
The wave-absorbing performance of the composite material is tested by using a vector network analyzer, and the result is shown in fig. 8. it can be seen that the graphene/amorphous titanium dioxide nanorod composite material prepared in the embodiment 4 has good wave-absorbing performance in a certain frequency range, when the thickness is 3.5mm, the minimum reflection loss reaches-41 dB at 8GHz, and when d is 2mm, the effective absorption band (R L < -10dB) width reaches 5GHz (13-18 GHz), and the graphene/amorphous titanium dioxide nanorod composite material is expected to be practically applied to a wave-absorbing coating material to realize the electromagnetic shielding performance of the coating material.
EXAMPLE 6 (crystalline TiO)2COMPARATIVE EXAMPLE
Taking 50mg of the composite material obtained in the embodiment 4, calcining the sample at 550 ℃ for 120min by using argon as a protective gas to obtain the graphene/crystalline titanium dioxide nanorod composite material. The annealed TiO can be derived by reference to the TEM diffractogram of FIG. 62A distinct lattice structure appears.
The wave-absorbing performance of the composite material was tested using a vector network analyzer, and the results are shown in fig. 9. It can be seen that, compared with the composite material prepared in example 4, the graphene/crystalline titanium dioxide nanorod composite material synthesized in example 5 has reduced wave-absorbing performance in each frequency band.
The above-mentioned embodiments only express the embodiments of the present invention, but not should be understood as the limitation of the scope of the invention patent, it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the concept of the present invention, and these all fall into the protection scope of the present invention.
Claims (8)
1. The graphene/amorphous titanium dioxide nanorod composite material is characterized in that graphene oxide and tetrabutyl titanate are used as raw materials, the graphene oxide is reduced into graphene through a one-step hydrothermal method, and meanwhile, titanium elements in the tetrabutyl titanate uniformly grow on two surfaces of a graphene sheet layer in the form of amorphous titanium dioxide nanorods under the action of a hydrothermal process, so that the graphene/amorphous titanium dioxide nanorod composite material is finally formed; wherein the length and the width of the graphene sheet layer in the obtained composite material are both 1-8 mu m, and the length of the amorphous titanium dioxide nanorod is 300-500 nm.
2. The preparation method of the graphene/amorphous titanium dioxide nanorod composite material of claim 1, wherein the preparation method is characterized in that graphene oxide and tetrabutyl titanate are converted into the graphene/amorphous titanium dioxide nanorod composite material through a one-step hydrothermal method, wherein amorphous titanium dioxide nanorods are uniformly dispersed on a graphene sheet layer; the method comprises the following steps:
uniformly dispersing graphene oxide in absolute ethyl alcohol serving as a solvent, performing ultrasonic treatment to uniformly disperse the graphene oxide, and then sequentially dropwise adding glycerol and tetrabutyl titanate, wherein the glycerol is used as a morphology control agent, and after the ultrasonic treatment, placing the mixed solution in a reaction kettle to perform hydrothermal reaction at the reaction temperature of 180 ℃ for 15 hours; carrying out alcohol suction filtration and freeze-drying to obtain the graphene/amorphous titanium dioxide nanorod composite material; graphene/amorphous titanium dioxide nanorod composite materials with different composite densities can be obtained by changing the adding proportion of the graphene oxide and the tetrabutyl titanate, so that the electromagnetic parameters of the composite materials are comprehensively adjusted, and the composite materials have high-efficiency electromagnetic wave absorption performance;
the mass ratio of the graphene oxide to the titanium element in the tetrabutyl titanate is 0.1-10: 1.
3. The preparation method of the graphene/amorphous titanium dioxide nanorod composite material according to claim 2, wherein the mass ratio of titanium elements in the graphene oxide and the tetrabutyl titanate is preferably 1-2: 1.
4. The method for preparing the graphene/amorphous titanium dioxide nanorod composite material according to claim 2, wherein the mass ratio of titanium elements in the graphene oxide and the tetrabutyl titanate is preferably 1: 1.
5. The method for preparing a graphene/amorphous titanium dioxide nanorod composite material as claimed in claim 2, 3 or 4, wherein in the suction filtration process, a polytetrafluoroethylene microporous filter membrane is used as the filter membrane.
6. The method for preparing the graphene/amorphous titanium dioxide nanorod composite material according to claim 2, 3 or 4, wherein the first ultrasonic time is 2 hours, and the second ultrasonic time is 20 minutes.
7. The preparation method of the graphene/amorphous titanium dioxide nanorod composite material according to claim 5, wherein the first ultrasonic time is 2 hours, and the second ultrasonic time is 20 minutes.
8. The application of the graphene/amorphous titanium dioxide nanorod composite material as claimed in claim 1, wherein the graphene/amorphous titanium dioxide nanorod composite material is applied to the field of electromagnetic wave absorption and serves as a wave-absorbing and electromagnetic shielding material.
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| CN113068390A (en) * | 2021-03-31 | 2021-07-02 | 燕山大学 | Two-dimensional magnetic Fe3GeTe2Composite material of nanosheet and graphene nanosheet as well as preparation method and application of composite material |
| CN114149786A (en) * | 2021-12-08 | 2022-03-08 | 陕西铁路工程职业技术学院 | Interface polarization enhanced TiO2Preparation method of/RGO wave-absorbing material |
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