CN115322409A - Three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with efficient sound absorption performance and preparation method thereof - Google Patents
Three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with efficient sound absorption performance and preparation method thereof Download PDFInfo
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- 239000004205 dimethyl polysiloxane Substances 0.000 title claims abstract description 103
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Abstract
The invention belongs to the field of sound absorption materials, and discloses a preparation method of a three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance. The three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material prepared by the invention can realize good sound absorption effect in a sound wave frequency range of 200-6400Hz, and particularly realize high-efficiency sound absorption in a medium-high frequency range of 2000-6400Hz. The three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material prepared by the invention has good hydrophobic property, and the water contact angle is 118.42-137.84 degrees.
Description
Technical Field
The invention belongs to the field of sound absorption materials, and relates to a three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance and a preparation method thereof.
Background
As an emerging material, graphene, a two-dimensional material with single-atom-thickness sheets, has many excellent performances compared with a natural material, but conventional two-dimensional graphene sheets are easy to agglomerate due to the effect of conjugated pi bonds. And after the concentration of the oxygen-containing functional groups in the graphene oxide reaches a critical point, all the sheet layers are mutually overlapped, and a stable three-dimensional structure is formed through self-assembly. The three-dimensional graphene foam not only inherits the excellent performance of the two-dimensional graphene, but also has the advantages of light weight and high porosity, and can bring various applications for controlling the size of the sound absorption material based on the unique cell structure of the three-dimensional graphene foam, and make it possible to directly control noise pollution by using the graphene aerogel. In the prior art, a graphene oxide solution is directly subjected to a hydrothermal reaction, or a graphene powder is subjected to heating welding in a plasma, high temperature or electric joule mode, but the graphene has the characteristics of porosity and brittleness, so that the problems of unstable form and low commercialization potential are also avoided while the graphene has the characteristics of an acoustic absorption structure, and part of preparation technologies need to be carried out in a high vacuum or inert gas atmosphere, so that a large-size structure is difficult to prepare. Through improving the foaming mode and compounding with macromolecular material, can obtain the graphene lamellar structure of effective stable overlap joint, it not only can strengthen the mechanical properties of graphite alkene, and the acoustic damping characteristic of macromolecular material itself also can further promote the sound absorption performance of material. The carbon nano tube is a one-dimensional quantum material with a special tubular structure, has excellent performances of low density, high strength, large specific surface area and the like, and when the carbon nano tube is introduced into the surface of the matrix of the composite material, the wettability between interfaces is improved, meanwhile, the carbon nano tube can be embedded into the filling phase, the bonding strength between the matrix and the filling phase is greatly enhanced, and the forced compatibility and the synergistic effect between the matrix and the filling phase are improved. In addition, the reduced graphene sheet layer, the carbon nano tube and the polydimethylsiloxane are all non-polar or low-polar materials, so that the three materials have good hydrophobic properties.
Disclosure of Invention
The invention aims to provide a preparation method of a three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance, which can realize good sound absorption effect in a sound wave frequency range of 200 to 6400Hz, and particularly realize high-efficiency sound absorption in a medium-high frequency range of 2000 to 6400Hz.
The technical scheme provided by the invention is as follows:
a preparation method of a three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance comprises the steps of carrying out magnetic stirrer and ultrasonic treatment on a graphene oxide solution and multi-walled carbon nano tubes to prepare a pre-foaming solution; adding ascorbic acid and octyl decyl glucoside into the pre-foaming liquid, fully and magnetically stirring to obtain three-dimensional graphene foam, and freezing and drying to obtain aerogel; and putting the aerogel into an impregnation liquid to obtain the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material, wherein the impregnation liquid is prepared by mixing and stirring n-hexane, polydimethylsiloxane and a polydimethylsiloxane curing agent.
Further, the index method of the graphene oxide solution is as follows: adding graphene oxide into deionized water, placing the mixture on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, taking down a beaker when the graphene oxide is dissolved and no obvious agglomeration exists in the solution, adjusting the pH value to 10 by using ammonia water, placing the beaker into a high-frequency ultrasonic cleaner, and performing ultrasonic treatment on the solution for more than 2 h to completely disperse graphene sheets, thereby preparing the graphene oxide solution.
Furthermore, the concentration of the graphene oxide solution is 6-12 mg/mL.
Further, the step of freezing and drying is as follows: and (3) sealing the three-dimensional graphene foam, putting the three-dimensional graphene foam into an 80 ℃ oven for reaction for 12 h, then putting the three-dimensional graphene foam into a refrigerator for freezing, and drying the obtained hydrogel in an oven at 40 ℃ for 24 h after the three-dimensional graphene foam is completely solidified to obtain the aerogel.
Further, completely immersing the aerogel into the impregnation liquid, repeatedly pouring the residual solution after impregnation on the surface of the aerogel to fully impregnate the aerogel after a large number of bubbles are not generated, and then heating and curing the aerogel in a 120 ℃ oven to obtain the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with the concentration of 2 h.
Further, placing the graphene oxide solution and the multi-walled carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, placing the mixture into an ultrasonic cleaner, and carrying out ultrasonic treatment for 10min to prepare a pre-foaming solution.
Further, ascorbic acid and octyl decyl glucoside are added into the prefoaming liquid, the prefoaming liquid is placed on a magnetic heating stirrer to be fully stirred at the rotating speed of 2500 rpm, and the stirring is stopped after the color of the solution is changed from black to uniform dark brown and the volume is obviously increased, so that the foaming is realized.
Further, the mass ratio of the graphene oxide to the multi-walled carbon nanotube is 1:8~1:3; the mass ratio of the ascorbic acid to the octyl decyl glucoside to the pre-foaming liquid is 1.2:1:51.5 to 53.
Further, the mass ratio of the normal hexane to the polydimethylsiloxane curing agent is 30 to 60:10:1.
further, a preparation method of the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance comprises the following specific steps:
(1) Preparing a graphene oxide solution: weighing 1.44g to 2.88g of graphene oxide in a beaker by using a precision electronic balance, adding 100 mL deionized water, placing the beaker on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, taking the beaker down when the graphene oxide is dissolved and no obvious agglomeration exists in the solution, adjusting the pH to 10 by using ammonia water, placing the beaker in a high-frequency ultrasonic cleaner, and performing ultrasonic treatment on the solution for more than 2 h to completely disperse graphene sheet layers to prepare a graphene oxide solution;
(2) Preparation of pre-foaming liquid: adding a graphene oxide solution obtained in the step (1) into a reaction kettle according to a mass ratio of the graphene oxide solution to the graphene oxide of 1:8~1: 3. weighing 0.075 g-0.4 g of multi-walled carbon nanotubes, then placing the multi-walled carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5 h to 1 h, placing the multi-walled carbon nanotubes in a high-frequency ultrasonic cleaner, and carrying out ultrasound for 10min, wherein the frequency range is 50 to 200kHZ, and preparing to obtain a pre-foaming liquid;
(3) Foaming: weighing 2.4 g ascorbic acid and 2.0 g octyldecyl glucoside, adding the ascorbic acid and the 2.0 zxft 3242 octyldecyl glucoside into the prefoaming liquid prepared in the step (2), placing the prefoaming liquid on a magnetic heating stirrer, fully stirring at the rotating speed of 2500 rpm, and stopping stirring after the color of the solution is changed from black to uniform dark brown and the volume is obviously increased, so as to realize foaming;
(4) Freezing and drying: sealing the beaker in the step (3), putting the beaker into an oven at 80 ℃ for reaction for 12 h, then putting the beaker into a refrigerator for freezing, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the hydrogel is completely solidified to obtain aerogel;
(5) Impregnating and curing polydimethylsiloxane: preparing n-hexane and polydimethylsiloxane into a uniform solution according to the proportion of 5-10g of polydimethylsiloxane in each 30g of n-hexane, and mixing the polydimethylsiloxane and a polydimethylsiloxane curing agent (hydrogenated silicone oil or di-tert-butyl peroxide) according to the mass ratio of 10:1, adding a curing agent, stirring uniformly, preparing to obtain a steeping liquor, completely immersing the aerogel obtained in the step (4) into the liquor, repeatedly pouring the residual liquor after soaking on the surface of the aerogel to fully soak the aerogel after a large number of bubbles do not appear in the aerogel, and then heating and curing in a 120 ℃ oven for 2 h to obtain the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material.
In the invention, the addition amount of the graphene oxide in the step (1) is 1.44g-2.88g, namely the concentration of the prepared graphene oxide solution is 6 mg/mL-12 mg/mL.
In the invention, the addition amount of the multi-walled carbon nanotube in the step (2) is 0.075g to 0.4g.
In the present invention, the polydimethylsiloxane described in the step (5) is added in an amount of 5 to 10g.
The invention also provides a three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material which is prepared by the method.
Advantageous effects
The invention discloses a three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance, wherein three-dimensional graphene foam with stable form is prepared by utilizing an improved ice crystal/bubble double-template method, and the carbon nano tube and polydimethylsiloxane are compounded by taking the three-dimensional graphene foam as a matrix, so that the sound absorption performance of the material is further improved, and a carbon-based aerogel material with high-efficiency sound absorption performance and good hydrophobic performance is prepared. According to the invention, the one-dimensional nano material carbon nano tube is added in the foaming process of the two-dimensional graphene sheet, so that the surface modification can be further carried out on the foam structure, and the sound absorption performance of the material is changed.
The three-dimensional graphene foam with stable form is prepared by adopting a simple improved ice crystal/bubble double-template method, has a uniform open-cell structure, can effectively absorb sound waves and can dissipate the sound waves through viscous resistance and skeleton vibration. The compounding of the carbon nano tube and the polydimethylsiloxane is carried out, the surface of the matrix is modified, and the high molecular polymer is introduced, so that a new sound wave dissipation way is added. The three-dimensional graphene/carbon nano/polydimethylsiloxane composite material prepared by the invention can realize good sound absorption effect within a sound wave frequency range of 200-6400Hz, and particularly can reach a sound absorption coefficient of more than 0.8 within a medium-high frequency range of 2000-6400Hz, so that high-efficiency sound absorption is realized. Compared with the existing porous sound absorption material, the porous sound absorption material has lighter weight and better sound absorption efficiency under the same thickness. The three-dimensional graphene/carbon nano/polydimethylsiloxane composite material prepared by the method has good hydrophobic property, and the water contact angle of the composite material is 118.42-137.84 degrees. The three-dimensional graphene/carbon nano/polydimethylsiloxane composite material prepared by the invention can be applied to the field of advanced sound absorption materials.
Drawings
Fig. 1 (a) is a scanning electron microscope image of a three-dimensional graphene/carbon nano/polydimethylsiloxane composite material prepared in example 1;
fig. 1 (b) is a partial enlarged view of a scanning electron microscope image of the three-dimensional graphene/carbon nano/polydimethylsiloxane composite material prepared in example 1.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to limit the scope of the present invention.
Example 1: the embodiment is a preparation method of a three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with efficient sound absorption performance, and the preparation method is carried out according to the following steps.
(1) Preparing a graphene oxide solution: weighing 1.92g of graphene oxide in a beaker by using a precision electronic balance, adding 100 mL deionized water, placing the beaker on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, taking the beaker down when the graphene oxide is dissolved and no obvious agglomeration exists in the solution, adjusting the pH value to 10 by using ammonia water, placing the beaker in a high-frequency ultrasonic cleaner, and performing ultrasonic treatment on the graphene oxide by more than 2 h to completely disperse graphene sheet layers to prepare a graphene oxide solution;
(2) Preparation of pre-foaming liquid: adding a graphene oxide solution obtained in the step (1) into a reaction kettle according to a mass ratio of the graphene oxide solution to the graphene oxide of 1: 8. after weighing 0.1g of multi-walled carbon nanotubes, putting the multi-walled carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, putting the multi-walled carbon nanotubes into a high-frequency ultrasonic cleaner, and carrying out ultrasound for 10min to prepare a pre-foaming liquid;
(3) Foaming: weighing 2.4 g ascorbic acid and 2.0 g octadecylglucoside, adding into the prefoaming liquid prepared in the step (2), placing on a magnetic heating stirrer, fully stirring at the rotating speed of 2500 rpm, stopping stirring after the color of the solution is changed from black to uniform dark brown and the volume is obviously increased, and realizing foaming;
(4) Freezing and drying: sealing the beaker in the step (3), putting the beaker into an oven at 80 ℃ for reaction for 12 h, then putting the beaker into a refrigerator for freezing, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the hydrogel is completely solidified to obtain aerogel;
(5) Impregnating and curing polydimethylsiloxane: preparing n-hexane and polydimethylsiloxane into a uniform solution according to the proportion that each 30g of n-hexane contains 10g of polydimethylsiloxane, wherein the mass ratio of the polydimethylsiloxane to the polydimethylsiloxane curing agent is 10: adding a polydimethylsiloxane curing agent according to the proportion of 1, uniformly stirring to obtain an impregnation solution, completely immersing the aerogel obtained in the step (4) into the solution, repeatedly pouring the residual solution after impregnation on the surface of the aerogel to fully impregnate the aerogel after a large number of bubbles do not appear in the aerogel, and then heating and curing 2 h in a 120 ℃ oven to obtain the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material named as GF-8/CNTs-8:1/PDMS. In this example, a comparative sample without PDMS for curing was prepared and named GF-8/CNTs-8:1 to verify the effect of PDMS composition on improving the sound absorption performance.
The invention has the advantages that: the invention adopts a simple improved ice crystal/bubble double-template method for foaming, and combines the carbon nano tube and the polydimethylsiloxane. As shown in fig. 1, the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material prepared by the invention is composed of a three-dimensional network structure formed by overlapping graphene sheet layers and a large number of holes in a microstructure, and the carbon nanotube is attached to the surface of the graphene sheet layer, so that a good infiltration effect is provided for the composition of polydimethylsiloxane and the three-dimensional graphene network structure. The black block-shaped modified aerogel foam can effectively absorb sound waves and dissipate the sound waves through viscous resistance, skeleton vibration and high-molecular viscoelasticity, so that high-efficiency sound absorption is realized. In addition, as the components of the composite material are all hydrophobic materials, the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the invention has good hydrophobic performance.
The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the invention can achieve the maximum sound absorption effect at 2380Hz under the test thickness of 20mm, can achieve more than 82% of sound absorption efficiency within the frequency range of 2380Hz to 6400Hz, and can achieve more than 90% of high-efficiency sound absorption performance. The sample has a contact angle of 128.09 degrees and has good hydrophobic property. The maximum sound absorption effect of the GF-8/CNTs-8:1 sample which is not compounded with PDMS reaches 86% at 3520Hz, and the high-efficiency sound absorption of more than 90% cannot be achieved within 200-6400 Hz. The performance of a comparison sample fully verifies that the sound absorption performance of the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the invention can be greatly improved by compounding PDMS
The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the invention can be applied to the field of advanced sound absorption materials.
Example 2: the embodiment is a preparation method of a three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with efficient sound absorption performance, and the preparation method is carried out according to the following steps.
(1) Preparing a graphene oxide solution: weighing 1.92g of graphene oxide in a beaker by using a precision electronic balance, adding 100 mL deionized water, placing the beaker on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, taking the beaker down when the graphene oxide is dissolved and no obvious agglomeration exists in the solution, adjusting the pH value to 10 by using ammonia water, placing the beaker in a high-frequency ultrasonic cleaner, and performing ultrasonic treatment on the graphene oxide by more than 2 h to completely disperse graphene sheet layers to prepare a graphene oxide solution;
(2) Preparation of pre-foaming liquid: adding a graphene oxide solution obtained in the step (1) into a reaction kettle according to a mass ratio of the graphene oxide solution to the graphene oxide of 1: 6. after weighing 0.13g of multi-walled carbon nanotubes, putting the multi-walled carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, putting the multi-walled carbon nanotubes into a high-frequency ultrasonic cleaner, and carrying out ultrasound for 10min to prepare a pre-foaming liquid;
(3) Foaming: weighing 2.4 g ascorbic acid and 2.0 g octadecylglucoside, adding into the prefoaming liquid prepared in the step (2), placing on a magnetic heating stirrer, fully stirring at the rotating speed of 2500 rpm, stopping stirring after the color of the solution is changed from black to uniform dark brown and the volume is obviously increased, and realizing foaming;
(4) Freezing and drying: sealing the beaker in the step (3), putting the beaker into an oven at 80 ℃ for reaction for 12 h, then putting the beaker into a refrigerator for freezing, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the hydrogel is completely solidified to obtain aerogel;
(5) Impregnating and curing polydimethylsiloxane: preparing n-hexane and polydimethylsiloxane into a uniform solution according to the proportion that each 30g of n-hexane contains 10g of polydimethylsiloxane, wherein the mass ratio of the polydimethylsiloxane to the polydimethylsiloxane curing agent is 10: adding a polydimethylsiloxane curing agent according to the proportion of 1, uniformly stirring to obtain an impregnation solution, completely immersing the aerogel obtained in the step (4) into the solution, repeatedly pouring the residual solution after impregnation on the surface of the aerogel to fully impregnate the aerogel after a large number of bubbles do not appear in the aerogel, and then heating and curing 2 h in a 120 ℃ oven to obtain the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material named as GF-8/CNTs-6:1/PDMS. In this embodiment, a comparative sample without carbon nanotubes is additionally prepared, named GF-8/PDMS, for verifying the effect of carbon nanotube composite on improving the acoustic absorption performance.
The three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material prepared by the invention can achieve the maximum sound absorption effect at 2240Hz under the test thickness of 20mm, can achieve more than 73% of sound absorption efficiency within the frequency range of 2240Hz to 6400Hz, and can achieve more than 90% of high-efficiency sound absorption performance. The sample has a contact angle of 130.30 degrees and has good hydrophobic property. The maximum sound absorption performance of the GF-8/PDMS sample without the carbon nano tube is 87% at 2520Hz, and the high-efficiency sound absorption of more than 90% can not be achieved within 200-6400 Hz. The performance of a comparison sample fully verifies that the compounding of the carbon nano tube can greatly improve the sound absorption performance of the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the invention
The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the invention can be applied to the field of advanced sound absorption materials.
Example 3: the embodiment is a preparation method of a three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with efficient sound absorption performance, and the preparation method is carried out according to the following steps.
(1) Preparing a graphene oxide solution: weighing 1.92g of graphene oxide in a beaker by using a precision electronic balance, adding 100 mL deionized water, placing the beaker on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, taking the beaker down when the graphene oxide is dissolved and no obvious agglomeration exists in the solution, adjusting the pH value to 10 by using ammonia water, placing the beaker in a high-frequency ultrasonic cleaner, and performing ultrasonic treatment on the graphene oxide by more than 2 h to completely disperse graphene sheet layers to prepare a graphene oxide solution;
(2) Preparation of pre-foaming liquid: adding a graphene oxide solution obtained in the step (1) into a reaction kettle according to the mass ratio of the graphene oxide solution to graphene oxide of 1: 4. after weighing 0.2g of multi-walled carbon nanotubes, putting the multi-walled carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, putting the multi-walled carbon nanotubes into a high-frequency ultrasonic cleaner, and carrying out ultrasound for 10min to prepare a pre-foaming liquid;
(3) Foaming: weighing 2.4 g ascorbic acid and 2.0 g octadecylglucoside, adding into the prefoaming liquid prepared in the step (2), placing on a magnetic heating stirrer, fully stirring at the rotating speed of 2500 rpm, stopping stirring after the color of the solution is changed from black to uniform dark brown and the volume is obviously increased, and realizing foaming;
(4) Freezing and drying: sealing the beaker in the step (3), putting the beaker into an oven at 80 ℃ for reaction for 12 h, then putting the beaker into a refrigerator for freezing, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the hydrogel is completely solidified to obtain aerogel;
(5) Impregnating and curing polydimethylsiloxane: preparing n-hexane and polydimethylsiloxane into a uniform solution according to the proportion that each 30g of n-hexane contains 10g of polydimethylsiloxane, wherein the mass ratio of the polydimethylsiloxane to the polydimethylsiloxane curing agent is 10: adding a polydimethylsiloxane curing agent according to the proportion of 1, uniformly stirring to obtain an impregnation solution, completely immersing the aerogel obtained in the step (4) into the solution, repeatedly pouring the residual solution after impregnation on the surface of the aerogel to fully impregnate the aerogel after a large number of bubbles do not appear in the aerogel, and then heating and curing 2 h in a 120 ℃ oven to obtain the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material named as GF-8/CNTs-4:1/PDMS.
The three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material prepared by the invention can achieve the maximum sound absorption effect at 2500Hz under the test thickness of 20mm, can achieve the sound absorption efficiency of more than 87% within the frequency range of 2500Hz to 6400Hz, and can achieve the high-efficiency sound absorption performance of more than 90%. The sample has a contact angle of 134.16 degrees and has good hydrophobic property.
The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the invention can be applied to the field of advanced sound absorption materials.
Example 4: the embodiment is a preparation method of a three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with efficient sound absorption performance, and the preparation method is carried out according to the following steps.
(1) Preparing a graphene oxide solution: weighing 1.92g of graphene oxide in a beaker by using a precision electronic balance, adding 100 mL deionized water, placing the beaker on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, taking the beaker down when the graphene oxide is dissolved and no obvious agglomeration exists in the solution, adjusting the pH value to 10 by using ammonia water, placing the beaker in a high-frequency ultrasonic cleaner, and performing ultrasonic treatment on the graphene oxide by more than 2 h to completely disperse graphene sheet layers to prepare a graphene oxide solution;
(2) Preparation of pre-foaming liquid: adding a graphene oxide solution obtained in the step (1) into a reaction kettle according to the mass ratio of the graphene oxide solution to graphene oxide of 1: 3. after weighing 0.27g of multi-walled carbon nanotubes, putting the multi-walled carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, putting the multi-walled carbon nanotubes into a high-frequency ultrasonic cleaner, and carrying out ultrasound for 10min to prepare a pre-foaming liquid;
(3) Foaming: weighing 2.4 g ascorbic acid and 2.0 g octadecylglucoside, adding into the prefoaming liquid prepared in the step (2), placing on a magnetic heating stirrer, fully stirring at the rotating speed of 2500 rpm, stopping stirring after the color of the solution is changed from black to uniform dark brown and the volume is obviously increased, and realizing foaming;
(4) Freezing and drying: sealing the beaker in the step (3), putting the beaker into an oven at 80 ℃ for reaction for 12 h, then putting the beaker into a refrigerator for freezing, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the hydrogel is completely solidified to obtain aerogel;
(5) Impregnating and curing polydimethylsiloxane: preparing n-hexane and polydimethylsiloxane into a uniform solution according to the proportion that each 30g of n-hexane contains 10g of polydimethylsiloxane, wherein the mass ratio of the polydimethylsiloxane to the polydimethylsiloxane curing agent is 10:1, adding a polydimethylsiloxane curing agent, uniformly stirring, preparing to obtain an impregnation liquid, completely immersing the aerogel obtained in the step (4) into the solution, repeatedly pouring the residual solution after impregnation on the surface of the aerogel to fully impregnate the aerogel after a large number of bubbles do not appear in the aerogel, and then heating and curing 2 h in a 120 ℃ oven to obtain the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material named as GF-8/CNTs-3:1/PDMS.
The three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material prepared by the invention can achieve the maximum sound absorption effect at 2120Hz under the test thickness of 20mm, can achieve more than 79% of sound absorption efficiency within the frequency range of 2120Hz to 6400Hz, and can achieve more than 90% of high-efficiency sound absorption performance. The sample has a contact angle of 137.40 degrees and has good hydrophobic property.
The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the invention can be applied to the field of advanced sound absorption materials.
In the above examples, the composite material was prepared into a cylindrical test specimen having a diameter of 30mm and a thickness of 20mm, and the sound absorption coefficient was measured using a resistance tube of the type Br ü el & Kj æ r4206 (test frequency range 100-6400 Hz) using a dual microphone and digital frequency analysis system; the water contact angle was measured for the above examples using a water contact angle tester.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. It will be readily apparent to those skilled in the art that various modifications can be made to the embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make modifications and alterations to the present invention in light of the present disclosure.
Claims (10)
1. A preparation method of a three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with efficient sound absorption performance is characterized in that a graphene oxide solution and a multi-walled carbon nano tube are subjected to magnetic stirrer and ultrasonic treatment to prepare a pre-foaming solution; adding ascorbic acid and octyl decyl glucoside into the pre-foaming liquid, fully and magnetically stirring to obtain three-dimensional graphene foam, and freezing and drying to obtain aerogel; and putting the aerogel into an impregnation liquid to obtain the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material, wherein the impregnation liquid is prepared by mixing and stirring n-hexane, polydimethylsiloxane and polydimethylsiloxane curing agent.
2. The method for preparing the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with high-efficiency sound absorption performance according to claim 1, wherein the index method of the graphene oxide solution is as follows: adding graphene oxide into deionized water, placing the mixture on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, taking down a beaker when the graphene oxide is dissolved and no obvious agglomeration exists in the solution, adjusting the pH value to 10 by using ammonia water, placing the beaker into a high-frequency ultrasonic cleaner, and performing ultrasonic treatment on the solution for more than 2 h to completely disperse graphene sheets, thereby preparing the graphene oxide solution.
3. The preparation method of the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with the efficient sound absorption performance according to claim 1, wherein the concentration of the graphene oxide solution is 6-12 mg/mL.
4. The preparation method of the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with high sound absorption efficiency according to claim 1, wherein the step of freezing and drying comprises the following steps: and (3) sealing the three-dimensional graphene foam, putting the three-dimensional graphene foam into an 80 ℃ oven for reaction for 12 h, then putting the three-dimensional graphene foam into a refrigerator for freezing, and drying the obtained hydrogel in an oven at 40 ℃ for 24 h after the three-dimensional graphene foam is completely solidified to obtain the aerogel.
5. The preparation method of the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with high-efficiency sound absorption performance according to claim 1, wherein the aerogel is completely immersed in the impregnation solution, after a large number of bubbles do not appear any more, the solution remained after the impregnation is repeatedly poured on the surface of the aerogel to be fully impregnated, and then the aerogel is heated and cured in an oven at 120 ℃ for 2 h to obtain the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material.
6. The preparation method of the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with the efficient sound absorption performance according to claim 1, wherein the preparation method comprises the steps of placing a graphene oxide solution and multi-wall carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5 to 1 hour, placing the mixture in an ultrasonic cleaner, and carrying out ultrasonic treatment for 10min to obtain a pre-foaming solution.
7. The preparation method of the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with high sound absorption performance according to claim 1, wherein ascorbic acid and octyl decyl glucoside are added into the pre-foaming solution, the pre-foaming solution is placed on a magnetic heating stirrer to be fully stirred at the rotating speed of 2500 rpm, and the stirring is stopped after the color of the solution is changed from black to uniform dark brown and the volume of the solution is obviously increased, so that foaming is realized.
8. The preparation method of the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with high-efficiency sound absorption performance according to claim 1, wherein the mass ratio of the graphene oxide to the multi-walled carbon nanotubes is 1:8~1:3; the mass ratio of the ascorbic acid to the octyl decyl glucoside to the pre-foaming liquid is 1.2:1:51.5 to 53.
9. The preparation method of the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with the efficient sound absorption performance according to claim 1, wherein the mass ratio of n-hexane to polydimethylsiloxane to the polydimethylsiloxane curing agent is 30 to 60:10:1.
10. a three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material, prepared by the method of any one of claims 1~9.
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