CN110698723B - Multifunctional anti-fatigue graphene composite sponge and preparation method and application thereof - Google Patents
Multifunctional anti-fatigue graphene composite sponge and preparation method and application thereof Download PDFInfo
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Abstract
A multifunctional anti-fatigue graphene composite sponge and a preparation method and application thereof are disclosed, wherein the preparation method comprises the following steps: performing thermal expansion, ultrasonic oscillation and drying on the graphite intercalation compound, grinding and uniformly mixing the obtained expanded graphene sheet and Triton, adding deionized water for mixing, and uniformly stirring to obtain a mixed solution; in the mixed solution, the mass percent of the expanded graphene sheets is 0.47-1.43 wt%; and immersing the sponge into the mixed solution, performing ultrasonic treatment until the sponge is completely saturated, and drying to obtain the multifunctional anti-fatigue graphene composite sponge. The prepared multifunctional anti-fatigue graphene composite sponge can be applied to the three fields of engineering monitoring, sound insulation and electrochemistry; the adopted non-chemically modified expanded graphene sheets are well combined in the sponge matrix and uniformly distributed, and the sheet structure of the expanded graphene sheets is maintained; the method is a synthetic method with low cost, high yield and easy large-scale production.
Description
Technical Field
The invention relates to the application fields of aerospace, sound insulation materials, engineering detection and the like, in particular to the technical field of a preparation method of a multifunctional application type composite material, and particularly relates to a multifunctional anti-fatigue graphene composite sponge as well as a preparation method and application thereof.
Background
With the diversification of the application field of materials, multifunctional materials become the development trend of new material research, however, the existing multifunctional materials cannot meet the requirements of monitoring, sound insulation and electrochemical performance. For example, in the field of engineering detection, the sensing material has a deformation detection function and a sound insulation and shock absorption auxiliary function, and has great development potential; in addition, the research of the super capacitor as an energy storage element on an aircraft as a battery is also very advanced, and the existing researchers use the super capacitor on the aircraft, however, the preparation of the flexible super capacitor is a research hotspot, and the flexible composite material capable of detecting capacitance change is expected to be developed in the future, so that the super capacitor can be applied to the fields of aircraft electric quantity monitoring and the like. Therefore, the preparation of the composite material with multiple functions is very important, and the development prospect is very wide for improving the material utilization rate and reducing the cost.
In recent years, due to the structural characteristics and properties of porosity, looseness and elasticity of the porous material, the porous material can be widely applied to the fields of wearable equipment, seawater purification, electronics and the like, so that the porous material can be used as a base material of a multifunctional material. The conductive filler is added into the porous material, so that the conductivity of the porous material can be improved on the aspect of maintaining the property of the porous material, and the prepared conductive porous material has a unique pore structure and excellent conductive characteristics, so that the conductive porous material has wider application prospects in the fields of electrochemistry, supercapacitors and microwave absorption. However, conductive porous materials also have a number of limitations. The porous material prepared by the traditional process, such as a polymer prepolymer curing method, an aerogel preparation method, a foaming agent foaming method and the like, has poor air permeability and low porosity, and after the porous material and the conductive filler are compounded, the pore size distribution and the filler distribution of the porous material are not uniform, or the bonding degree of the filler and a porous structure framework is weak, so that the performance of the multifunctional material is insufficient. In addition, the agglomeration of the filler in the matrix is important to study, so that the existing porous materials are not uniformly dispersed.
Therefore, the combination of the porous structure and the conductive filler has been studied. However, there are several key issues that prevent the practical use of these materials. This is because, since porous composites are mostly prepared by infiltration or coating methods, the binding capacity and dispersion degree of the filler to the matrix are limited, resulting in that the functionalization performance does not reach the desired level. In addition, many conductive porous materials have short fatigue test period and long tensile length, and cannot reach actual measurement values in service life.
The graphene is formed by a layer sp2Hybridized carbon atoms. Since 2004, extensive and intensive research has been conducted in various fields. The graphene has excellent mechanical properties, optical properties, electrical properties and thermal properties. The conductivity of the graphene can reach 1.5 multiplied by 105S/m is expected to be in the field of energy storage. However, the existing graphene has an agglomeration problem, and how to uniformly disperse the graphene in a substance to exert the performance of the graphene is a main research direction. In order to improve the dispersibility of graphene, most of graphene is oxidized to prepare graphene oxide, and the prepared graphene oxide has amphipathy due to a large number of functional groups on the surface and is easy to react with other substances, but the process for preparing the graphene oxide is complex and has high requirements.
Disclosure of Invention
Based on the problems faced by the application field, the invention provides a multifunctional anti-fatigue graphene composite sponge and a preparation method and application thereof. The method is a novel preparation method for combining the filler with the matrix through physical modification and reinforcement, is easy to operate, simple in process, excellent in material performance and wide in multifunctional application performance, realizes multiple purposes of one material to a certain extent, solves a series of problems of low conductivity, poor tensile and fatigue test effects and the like caused by poor combination degree of the filler matrix, and is expected to be applied to the wider technical field.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a multifunctional anti-fatigue graphene composite sponge comprises the following steps:
step (1): carrying out thermal expansion on the graphite intercalation compound, then carrying out ultrasonic oscillation, and drying to obtain an expanded graphene sheet;
step (2): grinding and uniformly mixing the expanded graphene sheet and polyethylene glycol octyl phenyl ether (Triton) to obtain a Triton modified expanded graphene sheet; wherein, according to the mass ratio: expanded graphene sheets: polyethylene glycol octyl phenyl ether (Triton) ═ 1: (8-10);
and (3): mixing the Triton modified expanded graphene sheets with deionized water, and uniformly stirring to obtain a mixed solution; in the mixed solution, the mass percentage of the expanded graphene sheet is 0.47wt% -1.43 wt%;
and (4): the porosity is 88.725% + -0.53% and the density is 15-17kg/m3And soaking the sponge with the diameter of 2 +/-0.2 mu m of the framework into the mixed solution, performing ultrasonic treatment until the sponge is completely saturated, and drying to obtain the multifunctional anti-fatigue graphene composite sponge.
In the step (1), after the graphite intercalation compound is thermally expanded for 2-3min at 700 ℃, the graphite intercalation compound is dried after being uniformly ultrasonically oscillated in an acetone solvent to obtain an expanded graphene sheet; the ultrasonic frequency is 100 KHz;
the prepared expanded graphene sheet is 3-5 layers of graphene, the thickness is less than 10nm, and the conductivity can reach 1400S/cm.
In the step (2), in the Triton-modified expanded graphene sheet, Triton is attached to the surface of the expanded graphene sheet, so that the hydrophilic performance of the graphene sheet is improved, and experiments prove that the suspension time of the unmodified graphene sheet in deionized water is 30min, the suspension time of the Triton-modified expanded graphene sheet in the deionized water is 5h, and the Triton-modified expanded graphene sheet is dispersed in an aqueous solution more uniformly.
In the step (2), the time for uniformly grinding and mixing is preferably 40min to 60 min.
In the step (3), the time for stirring is preferably 2 hours or more.
In the step (4), the sponge is melamine sponge or polyurethane sponge.
In the step (4), the ultrasonic frequency is preferably 100KHz, and the ultrasonic time is more than 10 h.
In the step (4), the drying temperature is preferably 70-80 ℃.
A multifunctional anti-fatigue graphene composite sponge is prepared by the preparation method.
In the prepared multifunctional anti-fatigue graphene composite sponge, the volume percentage of the expanded graphene sheets is 1.15-1.9 vol.%.
The multifunctional anti-fatigue graphene composite sponge has the tensile strength ranging from 0.129MPa to 0.232MPa and the elongation at break ranging from 5.667% to 17.22%, the stability is still kept over 98% through 20000 times of tensile cycle experiments, the conductivity range is 5.868S/cm to 12.077S/cm, the high-decibel noise absorption rate can reach 63.33%, the low-decibel noise absorption rate can reach 67.78%, and the specific capacitance range is 9.9F/g to 18.1F/g.
The application of the multifunctional anti-fatigue graphene composite sponge is used as a deformation sensor, a sound insulation material and a super capacitor in monitoring engineering materials.
Compared with the existing multifunctional anti-fatigue graphene composite sponge, the multifunctional anti-fatigue graphene composite sponge and the preparation method and application thereof have the advantages that:
the material is multipurpose, and the application in three fields of engineering monitoring, sound insulation and electrochemistry is realized; the expanded graphene sheets after non-chemical modification are well combined in the sponge matrix and are uniformly distributed; the electronic state of the graphene substrate can be modified through non-covalent functionalization, the conductivity of the graphene substrate can be adjusted, and the sheet structure of the graphene substrate can be maintained to a great extent; the method is a synthetic method with low cost, high yield and easy large-scale production, and has important contribution to industrial production.
The invention adopts the sponge with stable preparation process as the porous material, is different from the porous material prepared by the traditional catalytic process in that the cost is low, the efficiency is high, the large-scale production can be realized, and most importantly, the porosity is high, the pore size is uniform, and the framework size is smaller.
Drawings
Fig. 1 is a process schematic diagram of a preparation method of the multifunctional anti-fatigue graphene composite sponge of the invention;
fig. 2 is an SEM image analysis of the multifunctional fatigue-resistant graphene composite sponge prepared in example 2 of the present invention;
fig. 3 is an SEM image analysis of the multifunctional fatigue-resistant graphene composite sponge prepared in example 3 of the present invention;
fig. 4 is an SEM image analysis of the multifunctional fatigue-resistant graphene composite sponge prepared in example 4 of the present invention;
fig. 5 is a graph showing the conductivity change trend of the multifunctional anti-fatigue graphene composite sponge prepared in embodiments 2 to 8 of the present invention after a conductivity test experiment performed by using test example (1) under different graphene contents;
fig. 6 is a graph showing the variation trend of the tensile strength and the elongation at break of the multifunctional fatigue-resistant graphene composite sponge prepared in the embodiments 9 to 15 of the present invention under different graphene contents after the tensile test in the test example (2);
fig. 7 shows the resistance change rate of the multifunctional anti-fatigue graphene composite sponge prepared in embodiments 9 to 15 of the present invention, after a fatigue test using test example (2), under analysis of the content of 0.79 wt% graphene;
fig. 8(a) is a resistance change trend of the multifunctional fatigue-resistant graphene composite sponge prepared in embodiments 9 to 15 of the present invention under a graphene content of 0.79 wt% after bending experiments of 0 °, 45 °, 90 °, 135 °, and 180 ° performed by using test example (3);
(b) after the multifunctional fatigue-resistant graphene composite sponge prepared in the 9-15 embodiments of the invention is subjected to 0 °, 45 °, 90 °, 135 ° and 180 ° torsion tests by using the test example (3), the resistance change trend of the material is analyzed under the condition of 0.79 wt% of graphene content;
fig. 9 is a resistance change diagram of the multifunctional fatigue-resistant graphene composite sponge prepared in embodiments 2 to 8 of the present invention, after being subjected to a pressure-sensitive test using test example (1), under a pressure of 2.45KPa, 4.9KPa, and 12.25KPa at a graphene content of 0.79 wt%;
fig. 10 shows the resistance change rate of the multifunctional fatigue-resistant graphene composite sponge prepared in examples 9 to 15 of the present invention at 0.79 wt% of graphene content after deformation monitoring test using test example (3);
FIG. 11 is a graph of the sound absorption performance of the multifunctional fatigue-resistant graphene composite sponge prepared in examples 9-15 of the present invention at 0.79 wt% graphene content after sound absorption test using test example (4);
fig. 12 shows electrochemical properties of the multifunctional fatigue-resistant graphene composite sponge prepared in embodiments 16 to 22 of the present invention, after electrochemical testing in test example (5), under different graphene contents at scan rates of 100 mV/s;
fig. 13 shows the electrochemical performance of the multifunctional fatigue-resistant graphene composite sponge prepared in examples 16 to 22 of the present invention at different scanning rates with a graphene content of 1.27 wt% after electrochemical testing in test example (5);
fig. 14 shows electrochemical properties of the multifunctional fatigue-resistant graphene composite sponge prepared in examples 16 to 22 of the present invention, after electrochemical testing using test example (5), under different current densities and with a graphene content of 1.27 wt%;
fig. 15 shows specific capacitance electrochemical performance of the multifunctional fatigue-resistant graphene composite sponge prepared in examples 16 to 22 of the present invention after electrochemical testing using test example (5) and under the condition of graphene content of 1.27 wt%, the material is cycled 20000 times.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the following examples, the conductivity test instrument for the prepared multifunctional fatigue-resistant graphene composite sponge is a sheet resistance meter (Daming, DMR-1C), the range is 20 Ω (220VAC,0.1A), the sponge with the size of 2.0cm × 2.0cm × 0.25cm is flatly placed on an insulating desktop, the surface resistance of the sponge is measured by a probe of the sheet resistance meter from different positions, an average value is obtained, and conductivity data is obtained by conversion;
in the following embodiment, a pressure-sensitive testing instrument for the prepared multifunctional fatigue-resistant graphene composite sponge is a FLUKE2638 Ahydrasieres III data acquisition device, weights of 100g, 200g and 500g are sequentially placed on a sponge with the size of 2.0cm × 2.0cm × 0.25cm, and the resistance change is recorded;
in the following embodiment, the temperature influence experimental apparatus for the prepared multifunctional fatigue-resistant graphene composite sponge is a numerical control oven and a FLUKE2638 Ahydrasies III data acquisition device, the temperature is uniformly increased from 35 ℃ to 90 ℃, the temperature increase speed is 54.55 s/DEG C, and the resistance change in the temperature increase process is recorded;
in the following examples, the dimensions of a test piece for performing a series of test experiments of stretching, fatigue, bending, twisting, deformation monitoring, sound insulation and electrochemistry on the prepared multifunctional fatigue-resistant graphene composite sponge are 6.0cm × 2.0cm × 0.25 cm;
in the following embodiments, the prepared multifunctional fatigue-resistant graphene composite sponge is subjected to tensile and fatigue test by using a conventional tensile machine (GX-SF001, Shen zhen Share dinstrumement equipment co.LTD, China) and a FLUKE2638 aquariaries III data acquisition device, wherein the gauge length is 30mm, the inch distance is 2mm/min, the tensile frequency is 3.33Hz, and the tensile length is 0.5 mm;
in the following embodiment, the prepared multifunctional fatigue-resistant graphene composite sponge is subjected to bending, torsion and deformation monitoring tests, and the apparatus is a FLUKE2638 Ahydrasieres III data acquisition device;
in the following examples, the prepared multifunctional fatigue-resistant graphene composite sponge is subjected to sound insulation test software magicuseditorsoftware, a recorder and a music player are simultaneously placed in an empty dark room, a common sponge dark room and a composite material sponge dark room through the construction of the empty dark room, the common sponge dark room and the composite material sponge dark room, and then audio in MP3 format is processed and analyzed through the software;
in the following examples, the electrochemical testing apparatus for the prepared multifunctional fatigue-resistant graphene composite sponge is an electrochemical workstation (CHI660EB19038, Chen hua Instrument co., Shanghai, China).
In the following examples, the content of the expanded graphene sheet refers to the mass percentage content of the expanded graphene sheet in the mixed solution.
Example 1
A preparation method of the multifunctional anti-fatigue graphene composite sponge comprises the following steps of:
(1) thermally expanding the graphite intercalation compound at 700 ℃ for 3min, then ultrasonically oscillating the graphite intercalation compound in an acetone solvent uniformly, and drying to obtain expanded graphene sheets; the ultrasonic frequency is 100 KHz;
(2) according to the mass ratio of the expanded graphene sheet to the Triton, the expanded graphene sheet: triton ═ 1: 10, mixing, grinding for 40min to enable Triton to be attached to the surface of the graphene to the maximum extent to obtain a Triton modified expanded graphene sheet;
(3) mixing fully ground 0.5g of Triton modified expanded graphene sheets with 63mL of deionized water, and mechanically stirring for more than 2 hours to uniformly mix the sheets to obtain a mixed solution;
(4) the porosity was 88.725%, the density was 16kg/m3And putting melamine sponge with the framework diameter of 2 mu m into the mixed solution, carrying out ultrasonic treatment for 10 hours at the frequency of 100KHz to ensure that the Triton modified expanded graphene sheets in the mixed solution are fully immersed into the sponge, and then putting the sponge into a 75 ℃ drying oven for drying to obtain the multifunctional fatigue-resistant graphene composite sponge.
(5) Preparing the prepared multifunctional anti-fatigue graphene composite sponge into pieces with fixed sizes of 2.0cm multiplied by 0.25cm, and carrying out conductivity tests, pressure-sensitive experiments and temperature influence experiments;
(6) the prepared multifunctional anti-fatigue graphene composite sponge is prepared into a tensile test piece with the fixed size of 6.0cm multiplied by 2.0cm multiplied by 0.25cm, and the tensile, fatigue, bending, torsion, deformation monitoring, sound insulation and electrochemical series test experiments are carried out.
Example 2
A preparation method of a multifunctional anti-fatigue graphene composite sponge comprises the following steps:
(1) weighing 0.3g of graphite intercalation compound, putting the graphite intercalation compound into a constant-temperature muffle furnace at 700 ℃, heating and expanding, putting the graphite intercalation compound into a beaker, using acetone as a solvent, oscillating and dispersing the acetone to be uniform at an ultrasonic frequency of 100KHz by using an ultrasonic cleaning instrument, and finally putting the beaker into an electrothermal constant-temperature drying oven at 80 ℃ to evaporate the acetone to obtain the required uniform expanded graphene sheet;
(2) the 3mL of Triton was extracted with a syringe, and the obtained expanded graphene sheet and the extracted Triton sheet were placed in an agate mortar and ground clockwise for 40 minutes to obtain a Triton-modified expanded graphene sheet.
(3) Pouring the Triton modified expanded graphene sheets into 63mL of deionized water, and mechanically stirring for 2 hours to obtain a mixed solution with the mass fraction of the expanded graphene sheets being 0.47 wt%;
(4) soaking a melamine sponge material with the size of 2.0cm multiplied by 0.25cm in the mixed solution, performing ultrasonic treatment in an ultrasonic cleaning machine for 10 hours at the ultrasonic frequency of 100KHz, taking out the sponge, and drying in a 75 ℃ oven to obtain the multifunctional fatigue-resistant graphene composite sponge, wherein the thickness of the multifunctional fatigue-resistant graphene composite sponge is 0.25cm, and the volume percentage content of the expanded graphene sheets in the multifunctional fatigue-resistant graphene composite sponge is 1.1504 vol%.
An SEM image of the prepared multifunctional anti-fatigue graphene composite sponge is shown in figure 2, and can be obtained through the SEM image, graphene sheets are still uniformly attached to a sponge framework in a state of few layers under the action of 100KHz ultrasonic treatment, and the fact that the bonding degree is strong is proved; according to the literature: han, Q.Meng, X.Pan, T.Liu, S.Zhang, Y.Wang, S.Haridy, S.Araby, synthetic effect of graphene and carbon nanotube on lap guard length and electric conductivity of epoxy adhesives, Journal of Applied Polymer Science,136(2019). The method for verifying hydrophilicity was carried out by placing 0.1g of unmodified graphene and 0.1g of Triton-modified expanded graphene sheet in 100mL of deionized water, subjecting the mixture to ultrasonic treatment at a frequency of 100KHz for 2 hours, standing the mixture, and observing that the suspension time of the unmodified graphene sheet and the suspension time of the Triton-modified expanded graphene sheet are 30min and 5h after the same ultrasonic treatment for 2 hours.
Example 3
A preparation method of a multifunctional anti-fatigue graphene composite sponge comprises the following steps:
(1) weighing 0.4g of graphite intercalation compound, putting the graphite intercalation compound into a constant-temperature muffle furnace at 700 ℃, heating and puffing, putting the graphite intercalation compound into a beaker, using acetone as a solvent, oscillating and dispersing the mixture to be uniform through an ultrasonic cleaner at the ultrasonic frequency of 100KHz, and finally putting the mixture into an electrothermal constant-temperature drying oven at 80 ℃ to evaporate the acetone to obtain the required uniform expanded graphene sheet;
(2) and (3) extracting 4ml of graphene oxide by using a syringe, placing the graphene oxide and the prepared expanded graphene sheet in an agate mortar, and grinding the graphene oxide and the prepared expanded graphene sheet clockwise for 40 minutes to obtain the Triton modified expanded graphene sheet.
(3) Pouring the Triton modified expanded graphene sheets into 63mL of deionized water, and mechanically stirring for 2 hours to obtain a mixed solution with the mass fraction of the expanded graphene sheets being 0.63 wt%;
(4) soaking a melamine sponge material with the size of 2.0cm multiplied by 0.25cm in the mixed solution, performing ultrasonic treatment in an ultrasonic cleaning machine for 10 hours at the ultrasonic frequency of 100KHz, taking out the sponge, and drying in a 75 ℃ oven to obtain the multifunctional fatigue-resistant graphene composite sponge, wherein the thickness of the multifunctional fatigue-resistant graphene composite sponge is 0.25cm, and the volume percentage content of the expanded graphene sheets in the multifunctional fatigue-resistant graphene composite sponge is 1.1946 vol%.
An SEM image of the prepared multifunctional fatigue-resistant graphene composite sponge is shown in figure 3.
Example 4
A preparation method of a multifunctional anti-fatigue graphene composite sponge comprises the following steps:
(1) weighing 0.5g of graphite intercalation compound, putting the graphite intercalation compound into a constant-temperature muffle furnace at 700 ℃, heating and expanding, putting the graphite intercalation compound into a beaker, using acetone as a solvent, oscillating and dispersing the acetone to be uniform at an ultrasonic frequency of 100KHz by using an ultrasonic cleaning instrument, and finally putting the beaker into an electrothermal constant-temperature drying oven at 80 ℃ to evaporate the acetone to obtain the required uniform expanded graphene sheet;
(2) and (3) extracting 5ml of graphene oxide by using a syringe, placing the graphene oxide and the prepared expanded graphene sheet in an agate mortar, and clockwise grinding for 40 minutes to obtain the Triton modified expanded graphene sheet.
(3) Pouring the Triton modified expanded graphene sheets into 63mL of deionized water, and mechanically stirring for 2 hours to obtain a mixed solution with the mass fraction of the expanded graphene sheets being 0.79 wt%;
(4) soaking a melamine sponge material with the size of 2.0cm multiplied by 0.25cm in the mixed solution, performing ultrasonic treatment in an ultrasonic cleaning machine for 10 hours at the ultrasonic frequency of 100KHz, taking out the sponge, and drying in a 75 ℃ oven to obtain the multifunctional fatigue-resistant graphene composite sponge, wherein the thickness of the multifunctional fatigue-resistant graphene composite sponge is 0.25cm, and the volume percentage content of the expanded graphene sheets in the multifunctional fatigue-resistant graphene composite sponge is 1.2389 vol%.
An SEM image of the prepared multifunctional fatigue-resistant graphene composite sponge is shown in figure 4.
Example 5
A preparation method of a multifunctional anti-fatigue graphene composite sponge comprises the following steps:
(1) weighing 0.6g of graphite intercalation compound, putting the graphite intercalation compound into a constant-temperature muffle furnace at 700 ℃, heating and expanding, putting the graphite intercalation compound into a beaker, using acetone as a solvent, oscillating and dispersing the acetone to be uniform at an ultrasonic frequency of 100KHz by using an ultrasonic cleaning instrument, and finally putting the beaker into an electrothermal constant-temperature drying oven at 80 ℃ to evaporate the acetone to obtain the required uniform expanded graphene sheet;
(2) and (3) extracting 6ml of graphene oxide by using a syringe, placing the graphene oxide and the prepared expanded graphene sheet in an agate mortar, and grinding the graphene oxide and the prepared expanded graphene sheet clockwise for 40 minutes to obtain the Triton modified expanded graphene sheet.
(3) Pouring the Triton modified expanded graphene sheets into 63mL of deionized water, and mechanically stirring for 2 hours to obtain a mixed solution with the mass fraction of the expanded graphene sheets being 0.94 wt%;
(4) soaking a melamine sponge material with the size of 2.0cm multiplied by 0.25cm in the mixed solution, performing ultrasonic treatment in an ultrasonic cleaning machine for 10 hours at the ultrasonic frequency of 100KHz, taking out the sponge, and drying in a 75 ℃ oven to obtain the multifunctional fatigue-resistant graphene composite sponge, wherein the thickness of the multifunctional fatigue-resistant graphene composite sponge is 0.25cm, and the volume percentage content of the expanded graphene sheets in the multifunctional fatigue-resistant graphene composite sponge is 1.3716 vol%.
Example 6
A preparation method of a multifunctional anti-fatigue graphene composite sponge comprises the following steps:
(1) weighing 0.7g of graphite intercalation compound, putting the graphite intercalation compound into a constant-temperature muffle furnace at 700 ℃, heating and expanding, putting the graphite intercalation compound into a beaker, using acetone as a solvent, oscillating and dispersing the acetone to be uniform at an ultrasonic frequency of 100KHz by using an ultrasonic cleaning instrument, and finally putting the beaker into an electrothermal constant-temperature drying oven at 80 ℃ to evaporate the acetone to obtain the required uniform expanded graphene sheet;
(2) and (3) extracting 7ml of graphene oxide by using a syringe, placing the graphene oxide and the prepared expanded graphene sheet in an agate mortar, and grinding the graphene oxide and the prepared expanded graphene sheet clockwise for 40 minutes to obtain the Triton modified expanded graphene sheet.
(3) Pouring the Triton modified expanded graphene sheets into 63mL of deionized water, and mechanically stirring for 2 hours to obtain a mixed solution with the mass fraction of the expanded graphene sheets being 1.11 wt%;
(4) soaking a melamine sponge material with the size of 2.0cm multiplied by 0.25cm in the mixed solution, performing ultrasonic treatment in an ultrasonic cleaning machine for 10 hours at the ultrasonic frequency of 100KHz, taking out the sponge, and drying in a 75 ℃ oven to obtain the multifunctional fatigue-resistant graphene composite sponge, wherein the thickness of the multifunctional fatigue-resistant graphene composite sponge is 0.25cm, and the volume percentage content of the expanded graphene sheets in the multifunctional fatigue-resistant graphene composite sponge is 1.4159 vol%.
Example 7
A preparation method of a multifunctional anti-fatigue graphene composite sponge comprises the following steps:
(1) weighing 0.8g of graphite intercalation compound, putting the graphite intercalation compound into a constant-temperature muffle furnace at 700 ℃, heating and expanding, putting the graphite intercalation compound into a beaker, using acetone as a solvent, oscillating and dispersing the acetone to be uniform at an ultrasonic frequency of 100KHz by using an ultrasonic cleaning instrument, and finally putting the beaker into an electrothermal constant-temperature drying oven at 80 ℃ to evaporate the acetone to obtain the required uniform expanded graphene sheet;
(2) and (3) extracting 8ml of graphene oxide by using a syringe, placing the graphene oxide and the prepared expanded graphene sheet in an agate mortar, and grinding the graphene oxide and the prepared expanded graphene sheet clockwise for 40 minutes to obtain the Triton modified expanded graphene sheet.
(3) Pouring the Triton modified expanded graphene sheets into 63mL of deionized water, and mechanically stirring for 2 hours to obtain a mixed solution with the mass fraction of the expanded graphene sheets being 1.27 wt%;
(4) soaking a melamine sponge material with the size of 2.0cm multiplied by 0.25cm in the mixed solution, performing ultrasonic treatment in an ultrasonic cleaning machine for 10 hours at the ultrasonic frequency of 100KHz, taking out the sponge, and drying in a 75 ℃ oven to obtain the multifunctional fatigue-resistant graphene composite sponge, wherein the thickness of the multifunctional fatigue-resistant graphene composite sponge is 0.25cm, and the volume percentage content of the expanded graphene sheets in the multifunctional fatigue-resistant graphene composite sponge is 1.7699 vol%.
Example 8
A preparation method of a multifunctional anti-fatigue graphene composite sponge comprises the following steps:
(1) weighing 0.9g of graphite intercalation compound, putting the graphite intercalation compound into a constant-temperature muffle furnace at 700 ℃, heating and expanding, putting the graphite intercalation compound into a beaker, using acetone as a solvent, oscillating and dispersing the acetone to be uniform at an ultrasonic frequency of 100KHz by using an ultrasonic cleaning instrument, and finally putting the beaker into an electrothermal constant-temperature drying oven at 80 ℃ to evaporate the acetone to obtain the required uniform expanded graphene sheet;
(2) and (3) extracting 9ml of graphene oxide by using a syringe, placing the graphene oxide and the prepared expanded graphene sheet in an agate mortar, and grinding the graphene oxide and the prepared expanded graphene sheet clockwise for 40 minutes to obtain the Triton modified expanded graphene sheet.
(3) Pouring the Triton modified expanded graphene sheets into 63mL of deionized water, and mechanically stirring for 2 hours to obtain a mixed solution with the mass fraction of the expanded graphene sheets being 1.43 wt%;
(4) soaking a melamine sponge material with the size of 2.0cm multiplied by 0.25cm in the mixed solution, performing ultrasonic treatment in an ultrasonic cleaning machine for 10 hours at the ultrasonic frequency of 100KHz, taking out the sponge, and drying in a 75 ℃ oven to obtain the multifunctional fatigue-resistant graphene composite sponge, wherein the thickness of the multifunctional fatigue-resistant graphene composite sponge is 0.25cm, and the volume percentage content of the expanded graphene sheets in the multifunctional fatigue-resistant graphene composite sponge is 1.8141 vol%.
Example 9
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 2, except that:
in the step 4, the multifunctional fatigue-resistant graphene composite sponge with the thickness of 0.25cm is made into a tensile piece, the sponge size of the preparation method of the tensile piece is different, the content of other reagents is increased by 3 times in volume times, and the other steps are the same. The dimensions of the tensile member were 6.0cm by 2.0cm by 0.25 cm.
Example 10
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 3, except that:
in the step 4, the multifunctional fatigue-resistant graphene composite sponge with the thickness of 0.25cm is made into a tensile piece, the sponge size of the preparation method of the tensile piece is different, the content of other reagents is increased by 3 times in volume times, and the other steps are the same. The dimensions of the tensile member were 6.0cm by 2.0cm by 0.25 cm.
Example 11
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 4, except that:
in the step 4, the multifunctional fatigue-resistant graphene composite sponge with the thickness of 0.25cm is made into a tensile piece, the sponge size of the preparation method of the tensile piece is different, the content of other reagents is increased by 3 times in volume times, and the other steps are the same. The dimensions of the tensile member were 6.0cm by 2.0cm by 0.25 cm.
Example 12
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 5, except that:
in the step 4, the multifunctional fatigue-resistant graphene composite sponge with the thickness of 0.25cm is made into a tensile piece, the sponge size of the preparation method of the tensile piece is different, the content of other reagents is increased by 3 times in volume times, and the other steps are the same. The dimensions of the tensile member were 6.0cm by 2.0cm by 0.25 cm.
Example 13
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 6, except that:
in the step 4, the multifunctional fatigue-resistant graphene composite sponge with the thickness of 0.25cm is made into a tensile piece, the sponge size of the preparation method of the tensile piece is different, the content of other reagents is increased by 3 times in volume times, and the other steps are the same. The dimensions of the tensile member were 6.0cm by 2.0cm by 0.25 cm.
Example 14
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 7, except that:
in the step 4, the multifunctional fatigue-resistant graphene composite sponge with the thickness of 0.25cm is made into a tensile piece, the sponge size of the preparation method of the tensile piece is different, the content of other reagents is increased by 3 times in volume times, and the other steps are the same. The dimensions of the tensile member were 6.0cm by 2.0cm by 0.25 cm.
Example 15
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 8, except that:
in the step 4, the multifunctional fatigue-resistant graphene composite sponge with the thickness of 0.25cm is made into a tensile piece, the sponge size of the preparation method of the tensile piece is different, the content of other reagents is increased by 3 times in volume times, and the other steps are the same. The dimensions of the tensile member were 6.0cm by 2.0cm by 0.25 cm.
Example 16
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 2, except that:
in the step 4, when the multifunctional anti-fatigue graphene composite sponge with the thickness of 0.25cm is used for preparing an electrochemical performance test piece, the multifunctional anti-fatigue graphene composite sponge needs to be soaked in 1MNa2SO4After overnight in solution, the test could be carried out.
Example 17
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 3, except that:
in the step 4, when the multifunctional anti-fatigue graphene composite sponge with the thickness of 0.25cm is used for preparing an electrochemical performance test piece, the multifunctional anti-fatigue graphene composite sponge needs to be soaked in 1MNa2SO4After overnight in solution, the test could be carried out.
Example 18
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 4, except that:
in the step 4, when the multifunctional anti-fatigue graphene composite sponge with the thickness of 0.25cm is used for preparing an electrochemical performance test piece, the multifunctional anti-fatigue graphene composite sponge needs to be soaked in 1MNa2SO4After overnight in solution, the test could be carried out.
Example 19
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 5, except that:
in the step 4, when the multifunctional anti-fatigue graphene composite sponge with the thickness of 0.25cm is used for preparing an electrochemical performance test piece, the multifunctional anti-fatigue graphene composite sponge needs to be soaked in 1MNa2SO4After the solution was left overnight in the air,the test can be performed.
Example 20
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 6, except that:
in the step 4, when the multifunctional anti-fatigue graphene composite sponge with the thickness of 0.25cm is used for preparing an electrochemical performance test piece, the multifunctional anti-fatigue graphene composite sponge needs to be soaked in 1MNa2SO4After overnight in solution, the test could be carried out.
Example 21
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 7, except that:
in the step 4, when the multifunctional anti-fatigue graphene composite sponge with the thickness of 0.25cm is used for preparing an electrochemical performance test piece, the multifunctional anti-fatigue graphene composite sponge needs to be soaked in 1MNa2SO4After overnight in solution, the test could be carried out.
Example 22
A preparation method of a multifunctional anti-fatigue graphene composite sponge, which is the same as that in example 8, except that:
in the step 4, when the multifunctional anti-fatigue graphene composite sponge with the thickness of 0.25cm is used for preparing an electrochemical performance test piece, the multifunctional anti-fatigue graphene composite sponge needs to be soaked in 1MNa2SO4After overnight in solution, the test could be carried out.
Test example 1
A performance test of multi-functional antifatigue graphite alkene composite sponge, includes following several kinds of test methods:
it should be noted that the volume percentage of the expanded graphene sheets immersed in the sponge and the mass percentage of the expanded graphene sheets in the mixed solution are in the same increasing trend and are approximately proportional, and in the following test, the performance of the mixed solution is analyzed by using the mass percentage of the expanded graphene sheets in the mixed solution as a standard.
(1) Conductivity, pressure sensitive test
The conductivity of the multifunctional fatigue-resistant graphene composite sponge obtained by the methods of examples 2 to 8 was tested by using a sheet resistance meter (20 Ω range, 220VAC,0.1A), the conductivity change trend is shown in fig. 5, it can be known from fig. 5 that the conductivity of the multifunctional fatigue-resistant graphene composite sponge shows a fluctuation trend (fig. 5) with the increase of the filling amount of the expanded graphene sheets, and the conductivity of the multifunctional fatigue-resistant graphene composite sponge shows an upward trend when the expanded graphene sheets (GnPs) are between 0.47wt% and 0.79 wt% in the mixed solution. It is possible that the conductivity of the multifunctional fatigue-resistant graphene composite sponge increases as the content of GnPs increases because when the concentration of GnPs in a solution is low, agglomeration hardly occurs. When the content of GnPs is increased to a value (1.11 wt%), aggregation may be formed in the sponge matrix, resulting in non-uniform internal structure of the multifunctional fatigue-resistant graphene composite sponge, thereby affecting conductivity. When the component is more than 1.11 wt%, the conductivity gradually increases. It was analyzed that it is likely that the expanded graphene sheets in the solution were high, resulting in more agglomeration inside the sponge, thereby filling the sponge. Thus, a homogeneous conductive system is again formed, which again increases the conductivity. When the content of the filler expanded graphene sheet in the mixed solution is 0.79 wt%, the conductivity of the expanded graphene sheet reaches a peak value, and the conductivity is the best. The pressure sensitivity is tested by adopting weights of 50g, 100g and 200g, and experimental data are recorded to analyze the conductivity and resistance change of the material; after the pressure-sensitive test, the resistivity change of the multifunctional fatigue-resistant graphene composite sponge is shown in fig. 9, and it can be known from fig. 9 that the resistance change of the multifunctional fatigue-resistant graphene composite sponge is larger and larger along with the continuous increase of the pressure. The expected reason is that as the distance between the upper and lower layers of the conductive frame becomes shorter and shorter, denser conductive paths are formed at higher pressures due to the presence of transient pressure, resulting in greater deformation of the skeleton and thus greater resistance change at compressive pressure. The resistance change was the greatest at a load of 12.25 KPa. In addition, the resistance value of the multifunctional fatigue-resistant graphene composite sponge after springback is not obviously changed compared with the original resistance value, and the resistance value and the trend of the resistivity change curve are almost the same, which may reflect that the multifunctional fatigue-resistant graphene composite sponge has stable resistance and excellent pressure sensitivity in the experiment.
(2) Tensile and fatigue test
Obtained by carrying out the procedures of examples 9 to 15The obtained multifunctional anti-fatigue graphene composite sponge is subjected to tensile and fatigue tests by using a tensile testing machine, and test data are recorded to analyze the tensile strength, the elongation at break and the resistance change rate of the material, wherein the cycle number is 20000, the frequency is 3.33HZ, and the inch distance is 0.5 mm/min; the obtained variation trends of the tensile strength and the elongation at break are shown in fig. 6, and it can be known from fig. 6 that the tensile strength of the multifunctional fatigue-resistant nano graphene composite sponge can be improved by the higher GnPs filler, and the elongation at break or peak value is reduced along with the increase of the filler. The modified GnPs had a maximum tensile strength of 0.232MPa at 1.27 wt% of the composition, an increase of about 35%. The elongation at break of the multifunctional fatigue-resistant graphene composite sponge is obviously reduced along with the addition of the filler. When the concentration of GnPs is 1.27 wt%, the elongation at break of the modified GnPs is reduced by about 66.9%. The reduction is due to the strengthening effect of the graphene, namely the toughening and hardening effect of the matrix in the accumulation process of the nanosheets. As is clear from FIG. 6, there is a clear intersection between the two curves, i.e., the intersection at a GnPs concentration of 0.79 wt%. The result shows that the tensile strength and the elongation at break of the sample can meet the requirements at the same time under the sub-formula. The resistance change rate trend of the multifunctional fatigue-resistant graphene composite sponge is shown in FIG. 7, and from FIG. 7, it can be seen that Δ R/R0Gradual attenuation occurs but the range of variation is small. Compared with other experiments with less cycle times, the experiment adopts more cycle times, and can show the stability of the multifunctional anti-fatigue graphene composite sponge. Display of the enlarged image, lowest Δ R/R0-0.034 in the initial cycle (0-200 cycles) and-0.048 in the final cycle (19800-. The multifunctional anti-fatigue graphene composite sponge may not reach a stable state in the early stage, but the performance of the multifunctional anti-fatigue graphene composite sponge tends to be stable after the first 200 cycles. The relative resistance at 0% strain drops slightly, probably due to the formation of a stable conductive network during dynamic loading. At the later stage of 200 cycles, the multifunctional anti-fatigue graphene composite sponge slightly deforms after a large number of stretching cycles, so that the structure of the internal conductive network changes, and the resistance change rate gradually decreases. However, in this multifunctional fatigue resistant grapheneAfter the surface of the composite sponge is stretched, the consistent change of the resistance of the composite sponge can be maintained in thousands of cycles, which shows that the multifunctional fatigue-resistant graphene composite sponge serving as a pressure sensor has long service life, good durability and high reliability.
(3) Bending, torsion and deformation monitoring experiment
The multifunctional fatigue-resistant graphene composite sponge obtained by the method in the embodiment 9-15 is subjected to bending, twisting and deformation monitoring experiments manually, and experimental data is recorded to analyze the resistance and the change rate of the resistance of the multifunctional fatigue-resistant graphene composite sponge; after 0 °, 45 °, 90 °, 135 °, and 180 ° bending experiments, the resistance change trend of the multifunctional fatigue-resistant graphene composite sponge is shown in fig. 8(a) under the condition of 0.79 wt% of graphene content, and after 0 °, 45 °, 90 °, 135 °, and 180 ° torsion tests, the resistance change trend of the multifunctional fatigue-resistant graphene composite sponge is shown in fig. 8(b) under the condition of 0.79 wt% of graphene content, and it can be known from fig. 8 that the multifunctional fatigue-resistant graphene composite sponge has good elasticity, and the resistance change is obvious under different mechanical loads (bending and torsion). Fig. 8 shows the resistance change for different bend and twist angles. The multifunctional fatigue-resistant graphene composite sponge exhibits good flexibility, being able to withstand the above loads without experiencing permanent deformation (tearing). It can be clearly seen that the resistance decreases with increasing angle, which provides potential for angular deformation monitoring and provides potential for future applications in sensors, material deformation monitoring, etc. At 0.79 wt% of graphene content, the resistance change rate of the multifunctional fatigue-resistant graphene composite sponge can be seen in fig. 10, and when the iron ruler is in a neutral state, the resistance change is stable and is approximately 0. However, when the bending occurs, the resistance occurs, and the resistance signal shows a significant change (fluctuation). Therefore, the special response of the multifunctional fatigue-resistant graphene composite sponge to deformation provides a basis for the application of the composite material in the field of material engineering.
(4) Sound insulation experiment
The multifunctional fatigue-resistant graphene composite sponge obtained by the method in the embodiment 9-15 is placed in a darkroom by constructing three darkrooms (an empty darkroom, a pure sponge darkroom and a multifunctional fatigue-resistant graphene composite sponge darkroom), a music player is placed in the darkroom, an experiment is carried out by recording, the audio frequency is analyzed, and the wave absorption rate of an experimental data analysis material is recorded; under the content of 0.79 wt% of graphene, the sound absorption performance of the multifunctional anti-fatigue graphene composite sponge is shown in fig. 11, and the sound absorption effect of the multifunctional anti-fatigue graphene composite sponge can be known from fig. 11. And in high and low decibels, the sound absorption rate of the multifunctional anti-fatigue graphene composite sponge is higher than that of a pure sponge material. The irregular shape of the GnPs on the sponge framework is analyzed, so that the surface roughness of the GnPs is increased, a diffuse reflection effect (multi-directional scattering of reflected waves) is generated, and the sound absorption effect is promoted. It has therefore proven to be suitable for use in the field of sound attenuation. Most importantly, this feature is applicable to military vehicles (aircraft, submarines, etc.), where stealth is of paramount importance.
(5) Electrochemical experiments
The multifunctional fatigue-resistant graphene composite sponge obtained by the method in the embodiment 16-22 is combined into a sandwich structure by using two electrode sponges, two platinum sheets as current collectors and one filter paper as a separator for experiment, and experimental data is recorded to analyze the capacitance, specific capacitance, current density, charge-discharge time and cycle stability of the material. At the graphene content of 0.79 wt%, the electrochemical performance of the material is shown in fig. 12, 13, 14 and 15, and from the four graphs, it can be known that the CV curve is a straight line for the melamine sponge, which means that there is no electrochemical capacitance. In contrast, the CV curve of the multifunctional fatigue-resistant graphene composite sponge is similar to a leaf-shaped parallelogram, and has typical characteristics of a super capacitor. This property is contributed by GnPs because it has high conductivity and provides a fast electron transport pathway inside the electrode. Compared with other materials, the multifunctional anti-fatigue graphene composite sponge with the content of 1.27 wt% is large in area and highest in specific capacitance. The reason for this is that the pores between the high-fraction multifunctional fatigue-resistant graphene composite sponge particles are more, so that more electronic channels are formed in the sponge, and more interfaces are provided for energy conversion. For the multifunctional fatigue-resistant graphene composite sponge containing 0.79 wt% and 1.27 wt% of graphene, the specific capacitance values calculated by CV curves are 7.5F/g and 9.9F/g respectively. The performance of the multifunctional fatigue-resistant graphene composite sponge with the component of 1.27 wt% in the range of 20mV/s to 100mV/s is researched. The shape of the Cyclic Voltammetry (CV) curve at different scan rates was similar to a parallelogram. The CV curves calculated specific capacitances of 18.1F/g, 11.1F/g, and 9.9F/g, respectively, as the scan rate was increased from 20mV/s to 100 mV/s. With the increase of the scanning speed, the specific capacitance of the multifunctional anti-fatigue graphene composite sponge is slightly reduced. This ability to test rates against each other is caused by the arrangement of the different electrodes and the interconnecting pores, which make the electrode surfaces very susceptible to electrolyte ions during charging and discharging. The specific capacitances calculated from the charge-discharge curves were 15.8F/g, 15.0F/g, 12.0F/g, and 7.5F/g, respectively, at different current densities (0.5A/g to 5A/g). As can be seen from the graph, the discharge time decreases with increasing current density. It can be seen that the capacitance decreases with increasing scan rate or current density. This tendency is due to the fact that the electrode material cannot be charged immediately, since the proton diffusion in the electrode material is time-dependent. The specific capacitance ranges of the supercapacitors calculated using the CV map and the GCD were approximately the same. At 1.27 wt.%, the capacity retention of the multifunctional fatigue-resistant graphene composite sponge is 94.3%. The large-area interface between the electrode and the electrolyte has a porous structure, so that the multifunctional anti-fatigue graphene composite sponge has a larger capacitance. The porous structure is formed in the initial cycle, and the capacitance performance tends to be stable in the subsequent cycle. Long-term cycling experiments show that the supercapacitor taking the multifunctional fatigue-resistant graphene composite sponge as the active material has high stability, which is probably due to the fact that graphene has high structural integrity.
By measuring and analyzing the conductivity and the mechanical property, the multifunctional anti-fatigue graphene composite sponge with the comprehensive performance of 0.79 wt% is excellent, and from the microscopic angle of an SEM (scanning electron microscope) image, the multifunctional anti-fatigue graphene composite sponge with the content of 0.79 wt% is uniformly dispersed in a matrix and is free from agglomeration. The multifunctional anti-fatigue graphene composite sponge has good efficiency in monitoring material deformation, sound attenuation and supercapacitor application.
Compared with the characteristics of pure sponge, such as non-conductivity, low tensile strength and no capacitive performance, the multifunctional anti-fatigue graphene composite sponge prepared by the experiment has development prospects and advantages in the aerospace field, the sound insulation and wave absorption field and the electrochemical application field.
Claims (6)
1. The preparation method of the multifunctional anti-fatigue graphene composite sponge is characterized by comprising the following steps:
step (1): thermally expanding the graphite intercalation compound at 700 ℃ for 2-3min, then carrying out ultrasonic oscillation in an acetone solvent, and drying to obtain expanded graphene sheets; wherein the ultrasonic frequency is 100 KHz; the prepared expanded graphene sheet is 3-5 layers of graphene, the thickness is less than 10nm, and the conductivity can reach 1400S/cm;
step (2): grinding and uniformly mixing the expanded graphene sheet and polyethylene glycol octyl phenyl ether to obtain a Triton modified expanded graphene sheet; wherein, according to the mass ratio: expanded graphene sheets: polyethylene glycol octyl phenyl ether = 1: (8-10); grinding and mixing uniformly for 40-60 min;
and (3): mixing the Triton modified expanded graphene sheets with deionized water, and uniformly stirring to obtain a mixed solution; in the mixed solution, the mass percentage of the expanded graphene sheet is 0.47-1.43 wt%;
and (4): the porosity is 88.725% + -0.53% and the density is 15-17kg/m3Soaking sponge with the diameter of 2 +/-0.2 mu m of the framework into the mixed solution, performing ultrasonic treatment until the sponge is completely saturated, and drying to obtain the multifunctional anti-fatigue graphene composite sponge; wherein the ultrasonic frequency is 100KHz, and the ultrasonic time is more than 10 h;
in the multifunctional anti-fatigue graphene composite sponge, the volume percentage content of the expanded graphene sheets is 1.15-1.9 vol.%, the tensile strength of the multifunctional anti-fatigue graphene composite sponge is 0.129-0.232 MPa, the elongation at break is 5.667-17.22%, after 20000 times of stretching cycle experiments, the stability is still kept above 98%, the conductivity is 5.868S/cm-12.077S/cm, the high-decibel noise absorption rate can reach 63.33%, the low-decibel noise absorption rate can reach 67.78%, and the specific capacitance value is 9.9F/g-18.1F/g.
2. The preparation method of the multifunctional fatigue-resistant graphene composite sponge according to claim 1, wherein in the step (3), the stirring is performed for more than 2 hours.
3. The preparation method of the multifunctional fatigue-resistant graphene composite sponge according to claim 1, wherein in the step (4), the sponge is melamine sponge or polyurethane sponge.
4. The preparation method of the multifunctional fatigue-resistant graphene composite sponge as claimed in claim 1, wherein in the step (4), the drying temperature is 70-80 ℃.
5. A multifunctional anti-fatigue graphene composite sponge is characterized by being prepared by the preparation method of any one of claims 1 to 4.
6. The application of the multifunctional fatigue-resistant graphene composite sponge as claimed in claim 5, wherein the multifunctional fatigue-resistant graphene composite sponge is used as a deformation sensor, a sound insulation material and a super capacitor in monitoring engineering materials.
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