CN115322409B - Three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with efficient sound absorption performance and preparation method thereof - Google Patents
Three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with efficient sound absorption performance and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 197
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 134
- 239000004205 dimethyl polysiloxane Substances 0.000 title claims abstract description 102
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 title claims abstract description 102
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 61
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 57
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 57
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- -1 octyl decyl Chemical group 0.000 claims description 56
- 238000005187 foaming Methods 0.000 claims description 46
- 239000004964 aerogel Substances 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 34
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 29
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 28
- 239000006260 foam Substances 0.000 claims description 19
- 229960005070 ascorbic acid Drugs 0.000 claims description 16
- 235000010323 ascorbic acid Nutrition 0.000 claims description 16
- 239000011668 ascorbic acid Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 238000009210 therapy by ultrasound Methods 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 229940073499 decyl glucoside Drugs 0.000 claims description 13
- 239000000017 hydrogel Substances 0.000 claims description 12
- 238000005470 impregnation Methods 0.000 claims description 12
- 239000002048 multi walled nanotube Substances 0.000 claims description 12
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- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000007710 freezing Methods 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 2
- HEGSGKPQLMEBJL-RKQHYHRCSA-N octyl beta-D-glucopyranoside Chemical compound CCCCCCCCO[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O HEGSGKPQLMEBJL-RKQHYHRCSA-N 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims 1
- 229930182478 glucoside Natural products 0.000 claims 1
- 150000008131 glucosides Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 18
- 230000000694 effects Effects 0.000 abstract description 13
- 230000002209 hydrophobic effect Effects 0.000 abstract description 10
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 84
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 10
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
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- 238000013329 compounding Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000011358 absorbing material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
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- 238000001764 infiltration Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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- 239000000843 powder Substances 0.000 description 1
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- 229920002545 silicone oil Polymers 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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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 nano tube/polydimethylsiloxane composite material prepared by the method can achieve good sound absorption effect in the sound wave frequency range of 200-6400Hz, and particularly achieve high-efficiency sound absorption in the middle-high frequency range of 2000-6400 Hz. The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the method has good hydrophobic performance, 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, which is a two-dimensional material of a single-atom-thickness sheet layer, exhibits many excellent properties compared with a natural material, but conventional two-dimensional graphene sheets are susceptible to agglomeration due to the effect of conjugated pi bonds. After the concentration of oxygen-containing functional groups in the graphene oxide reaches a critical point, all the sheets 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 higher 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 the direct control of noise pollution by using the graphene aerogel is possible. The prior art adopts a method of directly carrying out hydrothermal reaction on graphene oxide solution or carrying out heating welding on graphene powder in a plasma, high temperature or electric joule mode, but the characteristics of porosity and brittleness of the graphene inevitably have the problems of unstable form and low commercialization potential while having the characteristics of an acoustic absorption structure, and part of preparation technology needs 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 the high polymer material, the effectively and stably lapped graphene lamellar structure can be obtained, the mechanical property of graphene can be enhanced, and the acoustic damping characteristic of the high polymer material can further improve the sound absorption performance of the material. The carbon nano tube is a one-dimensional quantum material with a special tubular structure, has the 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, and meanwhile, the carbon nano tube is also embedded into a filling phase, so that 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 sheets, the carbon nanotubes and the polydimethylsiloxane are all nonpolar or weakly polar materials, so that the three materials have good hydrophobic performance.
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 200-6400Hz, and particularly realize high-efficiency sound absorption in a middle-high frequency range of 2000-6400 Hz.
The technical scheme provided by the invention is as follows:
the preparation method of the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance comprises the steps of preparing graphene oxide solution and multi-wall carbon nano tubes through a magnetic stirrer and ultrasonic treatment to obtain a pre-foaming liquid; adding ascorbic acid and octyl decyl glucoside into the pre-foaming liquid, fully magnetically stirring to obtain three-dimensional graphene foam, and freezing and drying to obtain aerogel; and (3) putting the aerogel into an impregnating solution to obtain the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material, wherein the impregnating solution is prepared by mixing and stirring n-hexane, polydimethylsiloxane and polydimethylsiloxane curing agent.
Further, the index method of the graphene oxide solution comprises the following steps: adding graphene oxide into deionized water, placing the deionized water on a magnetic heating stirrer, fully stirring for 0.5-1 h, taking down a beaker when the graphene oxide is dissolved and no obvious caking exists in the solution, adjusting the pH to 10 by ammonia water, and placing the solution into a high-frequency ultrasonic cleaner to completely disperse graphene sheets by more than 2 h ultrasonic waves, so as to obtain the graphene oxide solution.
Further, the concentration of the graphene oxide solution is 6 mg/mL-12 mg/mL.
Further, the freezing and drying steps are as follows: and (3) sealing the three-dimensional graphene foam, then placing the three-dimensional graphene foam into an oven at 80 ℃ to react 12 h, then placing the three-dimensional graphene foam into a refrigerator to freeze, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the three-dimensional graphene foam is completely solidified to obtain the aerogel.
Further, the aerogel is completely immersed into the impregnating solution, after a large number of bubbles are no longer generated, the solution remained after the impregnation is repeatedly poured on the surface of the aerogel to enable the aerogel to be fully impregnated, and then the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material is obtained by heating and curing 2 h in a baking oven at 120 ℃.
Further, placing the graphene oxide solution and the multiwall carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5-1 h, and placing the mixture into an ultrasonic cleaner for ultrasonic treatment for 10min to obtain the pre-foaming liquid.
Further, ascorbic acid and octyl decyl glucoside are added into the pre-foaming liquid, and the pre-foaming liquid is placed on a magnetic heating stirrer to be fully stirred at the rotating speed of 2500 rpm, and after the color of the solution is changed from black to uniform dark brown and the volume of the solution is obviously increased, stirring is stopped, so that foaming is realized.
Further, the mass ratio of graphene oxide to multiwall carbon nanotubes is 1:8~1:3, a step of; the mass ratio of the ascorbic acid to the octyl glucoside to the pre-foaming liquid is 1.2:1: 51.5-53.
Further, the mass ratio of n-hexane, polydimethylsiloxane and polydimethylsiloxane curing agent is 30-60: 10:1.
further, the 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 graphene oxide solution: weighing 1.44 g-2.88 g of graphene oxide in a beaker by using a precision electronic balance, adding 100 mL deionized water, placing on a magnetic heating stirrer, fully stirring for 0.5 h-1 h, taking down the beaker when the graphene oxide is dissolved and no obvious caking exists in the solution, adjusting the pH to 10 by using ammonia water, and placing in a high-frequency ultrasonic cleaner for ultrasonic treatment of more than 2 h to completely disperse graphene sheets, thus preparing the graphene oxide solution;
(2) Preparation of a pre-foaming liquid: adding a mass ratio of graphene oxide to graphene oxide solution obtained in the step (1) is 1:8~1: 3. placing 0.075-0.4 g of weighed multiwall carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5-1 h, placing the mixture into a high-frequency ultrasonic cleaner, and performing ultrasonic treatment for 10min with the frequency range of 50-200 kHZ to obtain a pre-foaming liquid;
(3) Foaming: weighing 2.4 g ascorbic acid and 2.0 g octyl decyl glucoside, adding the ascorbic acid and the 2.0 octyl decyl glucoside into the pre-foaming liquid prepared in the step (2), placing the pre-foaming liquid on a magnetic heating stirrer, fully stirring at a 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) And (3) freezing and drying: sealing the beaker in the step (3), then placing the beaker in an oven at 80 ℃ to react for 12 h, then placing the beaker in a refrigerator to freeze, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the hydrogel is completely solidified to obtain aerogel;
(5) Impregnation curing of polydimethylsiloxane: preparing a uniform solution of n-hexane and polydimethylsiloxane according to the proportion of 5-10 g of polydimethylsiloxane in every 30g of n-hexane, and preparing a mixture of polydimethylsiloxane and polydimethylsiloxane curing agent (hydrogenated silicone oil or di-tert-butyl peroxide) according to the mass ratio of 10:1, uniformly stirring, preparing an impregnating solution, immersing the aerogel obtained in the step (4) into the solution completely, repeatedly pouring the solution remained 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 the aerogel in an oven at 120 ℃ 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 1.44 g-2.88 g, namely the concentration of the prepared graphene oxide solution is 6 mg/mL-12 mg/mL.
In the invention, the adding amount of the multiwall carbon nanotube in the step (2) is 0.075 g-0.4 g.
In the invention, the adding amount of the polydimethylsiloxane in the step (5) is 5-10 g.
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, which is prepared by an improved ice crystal/bubble double-template method to prepare three-dimensional graphene foam with stable morphology, and the three-dimensional graphene foam is used as a matrix to compound carbon nano tube and polydimethylsiloxane, 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 of the foam structure can be further modified, and the sound absorption performance of the material is changed.
The invention adopts a simple improved ice crystal/bubble double-template method to prepare the three-dimensional graphene foam with stable morphology, and the foam has a uniform open-cell structure, can effectively absorb sound waves and can carry out sound wave dissipation through viscous resistance and skeleton vibration. The composite 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 acoustic wave dissipation path is added. The three-dimensional graphene/carbon nano/polydimethylsiloxane composite material prepared by the method can realize good sound absorption effect in the sound wave frequency range of 200-6400Hz, and particularly can reach the sound absorption coefficient of more than 0.8 in the middle-high frequency range of 2000-6400 Hz, so that high-efficiency sound absorption is realized. Compared with the existing porous sound absorbing material, the porous sound absorbing material has lighter weight and better sound absorbing efficiency at the same thickness. The three-dimensional graphene/carbon nano/polydimethylsiloxane composite material prepared by the method has good hydrophobic performance, and the water contact angle is 118.42-137.84 degrees. The three-dimensional graphene/carbon nano/polydimethylsiloxane composite material prepared by the method can be applied to the field of advanced sound absorption materials.
Drawings
FIG. 1 (a) is a scanning electron micrograph of the three-dimensional graphene/carbon nano/polydimethylsiloxane composite prepared in example 1;
fig. 1 (b) is a partial enlarged view of a scanning electron micrograph of the three-dimensional graphene/carbon nano/polydimethylsiloxane composite prepared in example 1.
Detailed Description
The following examples are further illustrative of the invention and are not intended to limit the scope of the invention.
Example 1: the embodiment is a preparation method of a three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance, and the preparation method is carried out according to the following steps.
(1) Preparing graphene oxide solution: weighing 1.92g of graphene oxide in a beaker by using a precision electronic balance, adding 100 mL deionized water, placing on a magnetic heating stirrer, fully stirring for 0.5-1 h, taking down the beaker when the graphene oxide is dissolved and no obvious caking exists in the solution, adjusting the pH to 10 by using ammonia water, and placing in a high-frequency ultrasonic cleaner to carry out ultrasonic treatment of more than 2 h to completely disperse graphene sheets, so as to obtain a graphene oxide solution;
(2) Preparation of a pre-foaming liquid: adding a mass ratio of graphene oxide to graphene oxide solution obtained in the step (1) is 1: 8. placing 0.1g of weighed multiwall carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5-1 h, and placing the mixture into a high-frequency ultrasonic cleaner for ultrasonic treatment for 10min to obtain a pre-foaming liquid;
(3) Foaming: weighing 2.4 g ascorbic acid and 2.0 g octyl decyl glucoside, adding the ascorbic acid and the 2.0 octyl decyl glucoside into the pre-foaming liquid prepared in the step (2), placing the pre-foaming liquid on a magnetic heating stirrer, fully stirring at a 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) And (3) freezing and drying: sealing the beaker in the step (3), then placing the beaker in an oven at 80 ℃ to react for 12 h, then placing the beaker in a refrigerator to freeze, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the hydrogel is completely solidified to obtain aerogel;
(5) Impregnation curing of polydimethylsiloxane: the n-hexane and the polydimethylsiloxane are prepared into a uniform solution according to the proportion of 10g of polydimethylsiloxane in 30g of n-hexane, and the mass ratio of the polydimethylsiloxane to the polydimethylsiloxane curing agent is 10:1, adding a polydimethylsiloxane curing agent in a proportion, uniformly stirring, preparing to obtain an impregnating solution, completely immersing the aerogel obtained in the step (4) into the solution, repeatedly pouring the solution left after impregnation on the surface of the aerogel after a large number of bubbles do not appear in the aerogel, fully impregnating the aerogel, and heating and curing the aerogel in a baking oven at 120 ℃ for 2 h to obtain the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material named GF-8/CNTs-8:1/PDMS. A comparative sample without PDMS curing, named GF-8/CNTs-8:1, was additionally prepared in this example for verifying the effect of PDMS compounding on the improvement of sound absorption properties.
The invention has the advantages that: the invention adopts a simple modified ice crystal/bubble double-template method to foam, and combines the carbon nano tube and the polydimethylsiloxane. As shown in fig. 1, the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the invention is formed by a three-dimensional network structure formed by overlapping graphene sheets and a large number of holes on a microstructure, and carbon nano tubes are attached to the surfaces of the graphene sheets, so that a good infiltration effect is provided for the recombination of polydimethylsiloxane and the three-dimensional graphene network structure. The black blocky modified aerogel foam can effectively absorb sound waves and conduct sound wave dissipation through viscous resistance, skeleton vibration and high-molecular viscoelasticity, so that efficient sound absorption is achieved. 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 method can achieve the maximum sound absorption effect at 2380Hz under the test thickness of 20mm, can achieve the sound absorption efficiency of more than 82% in the frequency range of 2380 Hz-6400 Hz, and can achieve the high-efficiency sound absorption performance of more than 90%. The sample has a contact angle of 128.09 degrees and good hydrophobic property. The maximum sound absorption effect of GF-8/CNTs-8:1 samples without PDMS reaches 86% at 3520Hz, and high-efficiency sound absorption of more than 90% cannot be achieved within 200-6400 Hz. The performance of the comparative sample fully verifies that the PDMS composite 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 method 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 nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance, and the preparation method is carried out according to the following steps.
(1) Preparing graphene oxide solution: weighing 1.92g of graphene oxide in a beaker by using a precision electronic balance, adding 100 mL deionized water, placing on a magnetic heating stirrer, fully stirring for 0.5-1 h, taking down the beaker when the graphene oxide is dissolved and no obvious caking exists in the solution, adjusting the pH to 10 by using ammonia water, and placing in a high-frequency ultrasonic cleaner to carry out ultrasonic treatment of more than 2 h to completely disperse graphene sheets, so as to obtain a graphene oxide solution;
(2) Preparation of a pre-foaming liquid: adding a mass ratio of graphene oxide to graphene oxide solution obtained in the step (1) is 1: 6. placing 0.13g of weighed multiwall carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5-1 h, and placing the mixture into a high-frequency ultrasonic cleaner for ultrasonic treatment for 10min to obtain a pre-foaming liquid;
(3) Foaming: weighing 2.4 g ascorbic acid and 2.0 g octyl decyl glucoside, adding the ascorbic acid and the 2.0 octyl decyl glucoside into the pre-foaming liquid prepared in the step (2), placing the pre-foaming liquid on a magnetic heating stirrer, fully stirring at a 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) And (3) freezing and drying: sealing the beaker in the step (3), then placing the beaker in an oven at 80 ℃ to react for 12 h, then placing the beaker in a refrigerator to freeze, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the hydrogel is completely solidified to obtain aerogel;
(5) Impregnation curing of polydimethylsiloxane: the n-hexane and the polydimethylsiloxane are prepared into a uniform solution according to the proportion of 10g of polydimethylsiloxane in 30g of n-hexane, and the mass ratio of the polydimethylsiloxane to the polydimethylsiloxane curing agent is 10:1, adding a polydimethylsiloxane curing agent in a proportion, uniformly stirring, preparing to obtain an impregnating solution, completely immersing the aerogel obtained in the step (4) into the solution, repeatedly pouring the solution left after impregnation on the surface of the aerogel after a large number of bubbles do not appear in the aerogel, fully impregnating the aerogel, and heating and curing the aerogel in a baking oven at 120 ℃ for 2 h to obtain the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material named GF-8/CNTs-6:1/PDMS. In this example, a comparative sample of uncomplexed carbon nanotubes, designated GF-8/PDMS, was additionally prepared for verifying the effect of carbon nanotube compounding on the improvement of sound absorption properties.
The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the method can achieve maximum sound absorption effect at 2240Hz under the test thickness of 20mm, can achieve sound absorption efficiency of more than 73% in the frequency range of 2240 Hz-6400 Hz, and can achieve high-efficiency sound absorption performance of more than 90%. The sample has a contact angle of 130.30 degrees and good hydrophobic property. The GF-8/PDMS sample without the carbon nano tube has the maximum sound absorption performance reaching at 2520Hz of 87% and cannot reach more than 90% of high-efficiency sound absorption within 200-6400 Hz. The performance of the comparative 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 method 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 nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance, and the preparation method is carried out according to the following steps.
(1) Preparing graphene oxide solution: weighing 1.92g of graphene oxide in a beaker by using a precision electronic balance, adding 100 mL deionized water, placing on a magnetic heating stirrer, fully stirring for 0.5-1 h, taking down the beaker when the graphene oxide is dissolved and no obvious caking exists in the solution, adjusting the pH to 10 by using ammonia water, and placing in a high-frequency ultrasonic cleaner to carry out ultrasonic treatment of more than 2 h to completely disperse graphene sheets, so as to obtain a graphene oxide solution;
(2) Preparation of a pre-foaming liquid: adding a mass ratio of graphene oxide to graphene oxide solution obtained in the step (1) is 1: 4. placing 0.2g of weighed multiwall carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5-1 h, and placing the mixture into a high-frequency ultrasonic cleaner for ultrasonic treatment for 10min to obtain a pre-foaming liquid;
(3) Foaming: weighing 2.4 g ascorbic acid and 2.0 g octyl decyl glucoside, adding the ascorbic acid and the 2.0 octyl decyl glucoside into the pre-foaming liquid prepared in the step (2), placing the pre-foaming liquid on a magnetic heating stirrer, fully stirring at a 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) And (3) freezing and drying: sealing the beaker in the step (3), then placing the beaker in an oven at 80 ℃ to react for 12 h, then placing the beaker in a refrigerator to freeze, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the hydrogel is completely solidified to obtain aerogel;
(5) Impregnation curing of polydimethylsiloxane: the n-hexane and the polydimethylsiloxane are prepared into a uniform solution according to the proportion of 10g of polydimethylsiloxane in 30g of n-hexane, and the mass ratio of the polydimethylsiloxane to the polydimethylsiloxane curing agent is 10:1, adding a polydimethylsiloxane curing agent in a proportion, uniformly stirring, preparing to obtain an impregnating solution, completely immersing the aerogel obtained in the step (4) into the solution, repeatedly pouring the solution left after impregnation on the surface of the aerogel after a large number of bubbles do not appear in the aerogel, fully impregnating the aerogel, and heating and curing the aerogel in a baking oven at 120 ℃ for 2 h to obtain the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material named GF-8/CNTs-4:1/PDMS.
The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the method 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% in the frequency range of 2500 Hz-6400 Hz, and can achieve the high-efficiency sound absorption performance of more than 90%. The sample has a contact angle of 134.16 degrees and good hydrophobic property.
The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the method 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 nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance, and the preparation method is carried out according to the following steps.
(1) Preparing graphene oxide solution: weighing 1.92g of graphene oxide in a beaker by using a precision electronic balance, adding 100 mL deionized water, placing on a magnetic heating stirrer, fully stirring for 0.5-1 h, taking down the beaker when the graphene oxide is dissolved and no obvious caking exists in the solution, adjusting the pH to 10 by using ammonia water, and placing in a high-frequency ultrasonic cleaner to carry out ultrasonic treatment of more than 2 h to completely disperse graphene sheets, so as to obtain a graphene oxide solution;
(2) Preparation of a pre-foaming liquid: adding a mass ratio of graphene oxide to graphene oxide solution obtained in the step (1) is 1: 3. placing 0.27g of weighed multiwall carbon nanotubes on a magnetic heating stirrer, fully stirring for 0.5-1 h, and placing the mixture into a high-frequency ultrasonic cleaner for ultrasonic treatment for 10min to obtain a pre-foaming liquid;
(3) Foaming: weighing 2.4 g ascorbic acid and 2.0 g octyl decyl glucoside, adding the ascorbic acid and the 2.0 octyl decyl glucoside into the pre-foaming liquid prepared in the step (2), placing the pre-foaming liquid on a magnetic heating stirrer, fully stirring at a 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) And (3) freezing and drying: sealing the beaker in the step (3), then placing the beaker in an oven at 80 ℃ to react for 12 h, then placing the beaker in a refrigerator to freeze, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the hydrogel is completely solidified to obtain aerogel;
(5) Impregnation curing of polydimethylsiloxane: the n-hexane and the polydimethylsiloxane are prepared into a uniform solution according to the proportion of 10g of polydimethylsiloxane in 30g of n-hexane, and the mass ratio of the polydimethylsiloxane to the polydimethylsiloxane curing agent is 10:1, adding a polydimethylsiloxane curing agent in a proportion, uniformly stirring, preparing to obtain an impregnating solution, completely immersing the aerogel obtained in the step (4) into the solution, repeatedly pouring the solution left after impregnation on the surface of the aerogel after a large number of bubbles do not appear in the aerogel, fully impregnating the aerogel, and heating and curing the aerogel in a baking oven at 120 ℃ for 2 h to obtain the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material named GF-8/CNTs-3:1/PDMS.
The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the method can achieve maximum sound absorption effect at 2120Hz under the test thickness of 20mm, can achieve sound absorption efficiency of more than 79% in the frequency range of 2120 Hz-6400 Hz, and can achieve high-efficiency sound absorption performance of more than 90%. The sample has a contact angle of 137.40 degrees and good hydrophobic property.
The three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material prepared by the method 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 dual microphone and a digital frequency analysis system using a BrSel & Kj æ r4206 type impedance tube (test frequency range 100-6400 Hz); the above examples were subjected to water contact angle measurement using a water contact angle tester.
The embodiments are described above in order to facilitate the understanding and application of the present invention by those of ordinary skill in the art. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described 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, based on the present disclosure, should make improvements and modifications within the scope of the present invention.
Claims (8)
1. A preparation method of a three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance is characterized in that graphene oxide solution and multi-wall carbon nano tubes are subjected to magnetic stirrer and ultrasonic treatment to prepare a pre-foaming liquid; adding ascorbic acid and octyl decyl glucoside into the pre-foaming liquid, fully magnetically stirring to obtain three-dimensional graphene foam, and freezing and drying to obtain aerogel; putting aerogel into impregnating solution to obtain a three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material, wherein the impregnating solution is prepared by mixing and stirring n-hexane, polydimethylsiloxane and polydimethylsiloxane curing agent; the mass ratio of graphene oxide to the multiwall carbon nanotubes is 1:8~1:3, a step of; the mass ratio of the ascorbic acid to the octyl glucoside to the pre-foaming liquid is 1.2:1: 51.5-53; the mass ratio of n-hexane, polydimethylsiloxane and polydimethylsiloxane curing agent is 30-60: 10:1.
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 method for preparing the graphene oxide solution is as follows: adding graphene oxide into deionized water, placing the deionized water on a magnetic heating stirrer, fully stirring for 0.5-1 h, taking down a beaker when the graphene oxide is dissolved and no obvious caking exists in the solution, adjusting the pH to 10 by ammonia water, and placing the solution into a high-frequency ultrasonic cleaner to completely disperse graphene sheets by more than 2 h ultrasonic waves, so as to obtain the graphene oxide solution.
3. The preparation method of the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance, which is disclosed in claim 1, is characterized in that the concentration of graphene oxide solution is 6 mg/mL-12 mg/mL.
4. The method for preparing a three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with efficient sound absorption performance according to claim 1, wherein the step of freeze-drying is: and (3) sealing the three-dimensional graphene foam, then placing the three-dimensional graphene foam into an oven at 80 ℃ to react 12 h, then placing the three-dimensional graphene foam into a refrigerator to freeze, and drying the obtained hydrogel in the oven at 40 ℃ for 24 h after the three-dimensional graphene foam is completely solidified to obtain the aerogel.
5. 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 aerogel is completely immersed in the impregnating solution, after a large number of bubbles are no longer generated, the solution remained after the impregnation is repeatedly poured on the surface of the aerogel to fully impregnate the aerogel, and then the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material is obtained by heating and curing 2 h in a 120 ℃ oven.
6. The preparation method of the three-dimensional graphene/carbon nano tube/polydimethylsiloxane composite material with high-efficiency sound absorption performance, which is characterized in that graphene oxide solution and multi-wall carbon nano tube are placed on a magnetic heating stirrer and fully stirred for 0.5-1 h, and then placed in an ultrasonic cleaner for ultrasonic treatment for 10min to prepare a pre-foaming liquid.
7. The method for preparing the three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material with high-efficiency sound absorption performance according to claim 1, wherein ascorbic acid and octyldecyl glucoside are added into a pre-foaming liquid, and the pre-foaming liquid is placed on a magnetic heating stirrer to be fully stirred at a rotating speed of 2500 rpm, and 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 foaming is realized.
8. A three-dimensional graphene/carbon nanotube/polydimethylsiloxane composite material, characterized in that it is prepared by the method of any one of claims 1-7.
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