CN108620003B - Preparation method of stretchable MXene/graphene composite aerogel with high electromagnetic shielding effect - Google Patents
Preparation method of stretchable MXene/graphene composite aerogel with high electromagnetic shielding effect Download PDFInfo
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- CN108620003B CN108620003B CN201810514577.2A CN201810514577A CN108620003B CN 108620003 B CN108620003 B CN 108620003B CN 201810514577 A CN201810514577 A CN 201810514577A CN 108620003 B CN108620003 B CN 108620003B
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Abstract
The invention discloses a preparation method of a telescopic MXene/graphene composite aerogel with a high electromagnetic shielding effect. According to the invention, the reduced graphene oxide and the MXene dispersion liquid are uniformly mixed, the modifier is introduced, and finally the MXene/graphene composite aerogel with high electromagnetic shielding effect can be obtained through cold drying treatment, so that the stacking density of MXene is reduced, a new macroscopic morphology is constructed, the mechanical property is extremely excellent, the scalability is realized, and the application feasibility of MXene in the aerospace field is promoted.
Description
Technical Field
The invention belongs to the technical field of nano composite material preparation, and relates to a preparation method of MXene/graphene composite aerogel.
Background
MXene is a two-dimensional transition metal carbide or carbonitride with a structure similar to graphene, and is generally prepared by etching or stripping off the A layer elements in MXA phase. For the MAX phase, M refers to a transition metal element, A typically refers to a group IIIA, IVA element, and X refers to a carbon element or a nitrogen element.
MXene has excellent conductivity which is the same as that of graphene, is a novel two-dimensional material with metal conductivity and has extremely excellent electromagnetic shielding performance. However, the MXene material exists macroscopically in the form of powder or film, the structure is extremely compact, the density is high, the structure is extremely easy to damage, and the scalability is not realized, so that the application of MXene in the field of electromagnetic shielding is seriously influenced. Since it is generally desirable in practical applications that the electromagnetic shielding material is lighter and better, and has excellent mechanical properties, especially for the aerospace field. In addition, the flexibility of the MXene material is not as good as that of graphene, so that the graphene aerogel with a three-dimensional structure similar to graphene is difficult to form, but currently, people urgently want to find a method for constructing the MXene with the three-dimensional structure similar to graphene. It is known from a large number of reported literatures that the reduced graphene oxide is easy to form the graphene aerogel with three-dimensional morphology. And the surface of the reduced graphene oxide contains rich oxygen-containing functional groups, and strong electrostatic repulsion exists between layers, so that the aqueous dispersion of the reduced graphene oxide is a colloid with negative electricity, and can stably exist for several months without precipitation. MXene obtained by hydrofluoric acid etching also has hydrophilic groups such as hydroxyl group and epoxy group on the surface, and its aqueous dispersion is also negatively charged. Therefore, the reduced graphene oxide and MXene can be uniformly dispersed together, and stable colloid can be easily formed, so that favorable theoretical support is provided for constructing the light MXene/graphene composite aerogel.
Disclosure of Invention
In order to solve the problems that the common MXene material is high in density, easy to damage and incapable of having scalability and further application of the material in the field of electromagnetic shielding is limited, the invention provides a preparation method of a stretchable MXene/graphene composite aerogel with high electromagnetic shielding effect. According to the invention, the reduced graphene oxide and the MXene dispersion liquid are uniformly mixed, the modifier is introduced, and finally the MXene/graphene composite aerogel with high electromagnetic shielding effect can be obtained through cold drying treatment, so that the stacking density of MXene is reduced, a new macroscopic morphology is constructed, the mechanical property is extremely excellent, the scalability is realized, and the application feasibility of MXene in the aerospace field is promoted.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the stretchable MXene/graphene composite aerogel with the high electromagnetic shielding effect comprises the steps of compounding MXene and reduced graphene oxide, inducing the reduced graphene oxide and MXene by using a modifier, and forming the three-dimensional network-shaped composite aerogel with the rich pore structure by using a cold drying treatment means. The specific implementation steps are as follows:
step one, dispersing reduced graphene oxide in deionized water to obtain a reduced graphene oxide solution with the concentration of 4-10 mg mL-1Solution A of (1).
In the step, the reduced graphene oxide is a large single-layer reduced graphene oxide, and the size of the reduced graphene oxide is 2-5 microns.
Step two, the concentration is 1-3 mg mL-1Mixing the MXene dispersion liquid with the solution A according to the mass ratio of 1-10: 1 to obtain a mixed solution B.
In this step, the MXene dispersion is obtained by etching Ti with hydrofluoric acid3AlC2And then prepared.
And step three, carrying out magnetic stirring on the mixed solution B and then carrying out ultrasonic treatment to obtain a uniformly mixed solution C.
In the step, the rotating speed of the magnetic stirring is 200-600 r/min, and the duration time is 10-30 min.
In the step, the ultrasonic power is 100-300W, and the ultrasonic time is 10-30 min.
And step four, adding the modifier into the solution C, and performing magnetic stirring and ultrasonic treatment to obtain a solution D.
In this step, the modifier is one or a combination of dopamine, chitosan, cellulose nanofiber, sodium alginate and polyvinyl alcohol.
In the step, the amount of the modifier is 3-5 wt% of the solution D.
In the step, the rotating speed of the magnetic stirring is 200-600 r/min, and the duration time is 10-30 min.
In the step, the ultrasonic power is 100-300W, and the ultrasonic time is 10-30 min.
And step five, carrying out freeze drying on the solution D to obtain the MXene/graphene composite aerogel.
In the step, the temperature of the freeze drying is-50 to-80 ℃, and the time is 48 hours.
The prepared telescopic MXene/graphene composite aerogel can be applied to the field of electromagnetic shielding in the aspect of aerospace.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, by utilizing the characteristic that the reduced graphene oxide is easy to form a three-dimensional structure, the reduced graphene oxide and MXene are compounded, and the modifier is added, so that the MXene can be induced to form a three-dimensional network structure, the macro-stacking density of MXene materials is greatly reduced, the modifier can be wrapped by the large-sheet structure of the MXene and the reduced graphene oxide, so that the inherent high conductivity can be kept, the mechanical strength of the whole composite aerogel can be enhanced by the modifier, the excellent scalability can be given to the MXene and the reduced graphene oxide, the three-dimensional network MXene/graphene composite aerogel with good scalability can be finally constructed, a new MXene macro-stacking morphology can be created, and the application field of the MXene/graphene composite aerogel can be widened.
2. According to the invention, the graphene with excellent mechanical property is introduced into MXene, so that the application potential of MXene in the field of electromagnetic shielding can be further enhanced.
3. The method is extremely simple, the cost of the used raw materials is low, and the industrial batch production is extremely easy to realize.
4. Compared with the conventional graphene aerogel, the composite aerogel prepared by the invention has extremely excellent conductivity and scalability.
Drawings
Fig. 1 is an MXene/graphene composite aerogel sample with high electromagnetic shielding effect, which is prepared in example 1;
fig. 2 is a scanning electron microscope photograph of the scalable MXene/graphene composite aerogel with high electromagnetic shielding effect prepared in example 2;
fig. 3 is a graph of the electromagnetic shielding effectiveness of the scalable MXene/graphene composite with high electromagnetic shielding effect prepared in examples 1-3.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
the preparation method of the telescopic MXene/graphene composite aerogel with the high electromagnetic shielding effect provided by the embodiment is realized through the following steps:
step one, preparing reduced graphene oxide into the solution with the concentration of 4 mg mL-1The reduced graphene oxide solution of (a), solution a.
Step two, etching Ti by hydrofluoric acid3AlC2To prepare MXene dispersion, and its concentration was controlled to 1.5 mg mL with deionized water-1. Mixing MXene dispersion liquid with the solution A according to the mass ratio of 1:1 to obtain a solution B.
And step three, magnetically stirring the solution B line at the rotating speed of 600 r/min for 30min, and then carrying out ultrasonic treatment for 40 min to obtain a solution C, wherein the ultrasonic power is 200W.
And step four, dissolving polyvinyl alcohol in deionized water, adding the polyvinyl alcohol into the solution C according to the proportion of 5 wt%, magnetically stirring the solution C for 20min at the speed of 400 r/min, and then carrying out ultrasonic treatment for 10min at the ultrasonic power of 100W to obtain a composite solution D.
And step five, freezing and drying the uniformly mixed composite solution D at-60 ℃ for 48 hours to obtain the MXene/graphene composite aerogel.
Fig. 1 shows an MXene/graphene composite aerogel sample with high electromagnetic shielding effect prepared in this embodiment. As can be seen from fig. 1, the MXene/graphene composite aerogel prepared in this embodiment has excellent compressibility and elasticity.
Example 2:
the preparation method of the stretchable MXene/graphene composite aerogel with the high electromagnetic shielding effect provided by the embodiment is realized through the following steps:
step one, preparing reduced graphene oxide into 10 mg mL-1The reduced graphene oxide solution of (a), solution a.
Step two, etching Ti by hydrofluoric acid3AlC2Preparing MXene dispersion, and preparing the concentration by using deionized waterIs 3 mg mL-1. Mixing MXene dispersion liquid with the solution A according to the mass ratio of 1:2 to obtain a solution B.
And step three, magnetically stirring the solution B at the rotating speed of 300 r/min for 20min, and then performing ultrasonic treatment for 30min to obtain a solution C, wherein the ultrasonic power is 100W.
Step four, preparing a tris buffer solution with the pH value of 8.5, adding the solution C, uniformly stirring, adding 4 wt% of dopamine, magnetically stirring for 20min at 400 r/min, and performing ultrasonic treatment for 10min at 100W of ultrasonic power to obtain a composite solution D.
And step five, freezing and drying the uniformly mixed composite solution D at-80 ℃ for 48 hours to obtain the MXene/graphene composite aerogel.
Fig. 2 shows a scanning electron microscope photograph of the scalable MXene/graphene composite aerogel with high electromagnetic shielding effect prepared in this example. As can be seen from fig. 2, the MXene/graphene composite aerogel prepared in this embodiment has a three-dimensional network structure and a large pore size, which reaches hundreds of micrometers, so that it has a scalability similar to a sponge.
Example 3:
the preparation method of the telescopic MXene/graphene composite aerogel with the high electromagnetic shielding effect provided by the embodiment is realized through the following steps:
step one, preparing reduced graphene oxide into 6 mg mL-1The reduced graphene oxide solution of (a), solution a.
Step two, etching Ti by hydrofluoric acid3AlC2To prepare MXene dispersion, and its concentration was controlled to 2 mg mL with deionized water-1. Mixing MXene dispersion liquid with the solution A according to the mass ratio of 1:3 to obtain a solution B.
And step three, magnetically stirring the solution B at the rotating speed of 500 r/min for 10min, and then carrying out ultrasonic treatment for 30min to obtain a solution C, wherein the ultrasonic power is 150W.
And step four, adding 3 wt% of cellulose nano-fiber into the solution C, then magnetically stirring the solution C for 150min at 200 r/min, and then carrying out ultrasonic treatment for 200 min at 150W of ultrasonic power to obtain a composite solution D.
And step five, freeze-drying the uniformly mixed composite solution D at-70 ℃ for 48 hours to obtain the MXene/graphene composite aerogel.
Fig. 3 shows the electromagnetic shielding effectiveness of the scalable MXene/graphene composite with high electromagnetic shielding effect prepared in examples 1-3. As can be seen from fig. 3, as the addition amount of MXene increases, the electromagnetic shielding performance of the obtained composite aerogel increases. The electromagnetic shielding performance of the composite aerogel obtained in the embodiment 1 can reach 20-25 dB, which is far higher than the minimum requirement for the electromagnetic shielding performance in practical application. The electromagnetic shielding effectiveness of the composite aerogel obtained in the embodiment 3 is as high as 30-50 dB, so that the composite aerogel has great potential in the electromagnetic shielding application field in the aspect of aerospace.
Claims (8)
1. A preparation method of a telescopic MXene/graphene composite aerogel with high electromagnetic shielding effect is characterized by comprising the following steps:
step one, dispersing reduced graphene oxide in deionized water to obtain a reduced graphene oxide solution with the concentration of 4-10 mg mL-1Solution A of (1);
step two, the concentration is 1-3 mg mL-1Mixing the MXene dispersion liquid with the solution A according to the mass ratio of 1-10: 1 to obtain a mixed solution B;
step three, carrying out magnetic stirring on the mixed solution B and then carrying out ultrasonic treatment to obtain a uniformly mixed solution C;
adding a modifier into the solution C, performing magnetic stirring and ultrasonic treatment to obtain a solution D, wherein the modifier is one or a combination of dopamine, chitosan, cellulose nanofiber, sodium alginate and polyvinyl alcohol;
and step five, carrying out freeze drying on the solution D to obtain the MXene/graphene composite aerogel.
2. The preparation method of the MXene/graphene composite aerogel with high electromagnetic shielding effect as claimed in claim 1, wherein the reduced graphene oxide is a large single layer of reduced graphene oxide with a size of 2-5 μm.
3. The method for preparing the MXene/graphene composite aerogel with high electromagnetic shielding effect as claimed in claim 1, wherein the MXene dispersion is obtained by etching Ti with hydrofluoric acid3AlC2And then prepared.
4. The preparation method of the MXene/graphene composite aerogel with high electromagnetic shielding effect as claimed in claim 1, wherein the rotation speed of the magnetic stirring in the third step and the fourth step is 200-600 r/min, and the duration time is 10-30 min.
5. The preparation method of the MXene/graphene composite aerogel with high electromagnetic shielding effect as claimed in claim 1, wherein in the third step and the fourth step, the ultrasonic power is 100-300W, and the ultrasonic time is 10-30 min.
6. The preparation method of the MXene/graphene composite aerogel with high electromagnetic shielding effect as claimed in claim 1, wherein the amount of the modifier is 3-5 wt% of the solution D.
7. The preparation method of the MXene/graphene composite aerogel with high electromagnetic shielding effect as claimed in claim 1, wherein the temperature of freeze drying is-50 to-80 ℃ and the time is 48 h.
8. The MXene/graphene composite aerogel with high electromagnetic shielding effect prepared by the method of any one of claims 1 to 7 is applied to the field of electromagnetic shielding in aerospace.
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