CN116178959A - Graphene acousto-electric signal conversion film, preparation method, detector and sensing device - Google Patents
Graphene acousto-electric signal conversion film, preparation method, detector and sensing device Download PDFInfo
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Abstract
The invention belongs to the technical field of acoustic-electric signal conversion materials, and discloses a graphene acoustic-electric signal conversion film, a preparation method, a detector and a sensing device. Using a single layer or a few layers of Mxene as a reinforcing phase, mixing the reinforcing phase with graphene oxide in a solution mode, and obtaining Mxene reinforced graphene through hydrothermal reaction; and mixing the Mxene reinforced graphene with an elastic polymer monomer, performing in-situ shrinkage polymerization on the elastic polymer monomer, and performing suction filtration to form a film to obtain the Mxene reinforced graphene elastic polymer film. The micro-acoustic sensor detector manufactured by utilizing the MXene reinforced graphene film has the mechanical properties of high strength and high toughness, the frequency response range of the detector is obviously improved, the frequency response time is shortened, and the sensitivity is improved. The invention can not only improve the structural stability of graphene, but also improve the sensitivity of the film to vibration signals by utilizing the two-dimensional conductive thin layer structure of Mxene.
Description
Technical Field
The invention belongs to the technical field of acoustic-electric signal conversion materials, and particularly relates to a graphene acoustic-electric signal conversion film, a preparation method, a detector and a sensing device.
Background
Sound propagation causes sound pressure changes in the air and is fast, and weak sound pressure fluctuations are hidden in the thermal motion of the gas molecules. It is very difficult to acquire a weak sound signal by directly detecting a weak sound pressure change in the air, and a conventional pickup records sound by recording vibration of a diaphragm under a sound pressure load. Obviously, the ability to detect weak sound pressure variations in air is inseparable from the ability to detect bending deformations (bending stiffness) of the membrane. When the sound pressure is weak enough to cause the diaphragm to bend and deform recognizable, even if a power amplifier is used, a weak sound signal that is not captured cannot be amplified. The traditional pickup uses metal films as diaphragms to sense sound pressure, and the diaphragms have certain thickness, so the diaphragms have certain bending rigidity, and weak sound pressure load can not cause the diaphragms to bend and deform, so weak sound can not be recorded. If the diaphragm structure of the pickup can be made of thinner film material with smaller bending stiffness, a weaker sound can be recorded.
Because graphene has very high in-plane stretching strength, extremely low bending rigidity and excellent mechanical and electrical properties, the graphene has a wide application prospect in the field of acoustic mechanics and is a hotspot for application research of graphene.
The field grass and the like research a single-layer graphene sound source device, transfer single-layer graphene to an alumina electrode, and enable the single-layer graphene to generate sound in a suspending manner. Then, performances of the single-layer graphene and the multi-layer graphene are compared through theory and experiment, and a graphene sound source device based on the PET transparent substrate is prepared and tested.
Yan Shanda and the like develop a flexible graphene piezoresistive sensor, and a graphene voice detection sensor with a cylindrical micro-surface structure substrate is prepared by a team through a Chemical Vapor Deposition (CVD) in-situ template method and an imprinting technology aiming at the problem that traditional voice acquisition and recognition are easily affected by environmental noise.
Professor Yan Shankai, et al, incorporated a multi-layered graphene film (MGM) into the tympanic membrane for wideband hearing recovery in rats, MGM showed good biocompatibility and biostability, promoted growth of tympanic membrane cells in a regulated manner, with little evidence of tissue rejection and inflammatory response. Wideband hearing recovery (1-32 kHz) can be achieved and maintained for at least 2 months. Mechanical simulations indicate that the high elastic modulus of MGM and the thin thickness of the reconstructed tympanic membrane play a key role in high frequency hearing recovery.
The professor Des Gibson, university of scotland thin film sensor imaging research institute, et al, demonstrates the use and applicability of ultra-thin graphene foam (GRF) employing Polydimethylsiloxane (PDMS) embedded in the GRF structure as an active layer in a piezoresistive pressure sensor for robotic touch sensing applications. It is worth noting that GRF/PDMS-GRF is composed of only a few layers of graphene, can show sensitivity to pressure in the range of 0 to 100kPa, and solves the difficulty that the current robot lacks of realizing touch and tactile feedback.
Light layered three-dimensional graphene aerogels (LGAs) with highly elastic conductive networks were prepared by bi-directional freezing of graphene oxide aqueous suspensions, followed by lyophilization and thermal annealing, as taught by the university of beijing chemistry, inc. Due to the laminated structure of the LGA, the compressive strength of the LGA along the direction vertical to the laminated surface is far lower than that of isotropic and unidirectional oriented graphene aerogel with similar apparent density, so that the LGA has ultrahigh sensitivity of 3.69kPa and low detection limit of 0.15Pa, and the LGA can be used normally in extreme environments and can detect dynamic force frequency and sound vibration, and is very effective in detecting biological signals of wrist pulse and finger bending.
Through the above analysis, the problems and defects existing in the prior art are as follows: the graphene film used in the prior art is mainly prepared by adopting a Chemical Vapor Deposition (CVD) method, the preparation cost of the graphene film by the CVD method is high, the growth process is complex, and the quality of the obtained graphene film is difficult to control. And is extremely fragile during the transfer of graphene. The graphene oxide is used as a raw material, and the graphene film obtained through film formation reduction has the problems of easiness in layering, unstable structure and the like, and is easy to generate irreversible random fracture inside the graphene film, so that the stability and the reliable acousto-electric signal conversion of the graphene film are affected.
Disclosure of Invention
In order to overcome the problems in the related art, the embodiment of the invention discloses a graphene acousto-electric signal conversion film, a preparation method, a detector and a sensing device. In particular to a graphene acousto-electric signal conversion film based on Mxene enhancement.
The technical scheme is as follows: the graphene acousto-optic signal conversion film based on Mxene enhancement is characterized in that the film converts vibration acoustic signals into electric signals of multiple orders of magnitude by using a distributed Mxene enhanced graphene conductive network.
In one embodiment, the Mxene-enhanced graphene conductive network is an Mxene-enhanced two-dimensional conductive thin layer structure.
The invention further aims to provide a preparation method for realizing the graphene acousto-optic signal conversion film based on Mxene enhancement, which comprises the following steps:
step one, preparing a single-layer few-layer Mxene material;
step two, using an Mxene material as a reinforcing phase, mixing the reinforcing phase with graphene oxide in a solution mode, and obtaining the Mxene reinforced graphene through a hydrothermal reaction;
and thirdly, mixing the Mxene reinforced graphene with an elastic polymer monomer, and performing in-situ shrinkage polymerization on the elastic polymer monomer, and performing suction filtration to form a film to obtain the Mxene reinforced graphene elastic polymer film.
In one embodiment, in step one, the preparation of the Mxene material comprises:
adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:10-40, the HCl concentration in the HCl solution is 9M & mol/L, and the stirring time is 20-120min;
ti is mixed with 3 AlC 2 Adding the powder into the mixed solution in batches and fully stirring for reaction; ti (Ti) 3 AlC 2 The proportion of the mixed solution is 1:10-100, wherein the reaction temperature is 20-60 ℃ and the reaction time is 12-48h;
after complete reaction, deionized water is added for washing until the pH value is 7; adding ethanol for cleaning, centrifuging at 10000r/min for 10min to remove supernatant, adding deionized water again, and centrifuging at 3500r/min for 3min to obtain MXene supernatant.
In one embodiment, in step two, the preparation of Mxene enhanced graphene comprises the steps of:
mixing graphene oxide dispersion liquid and Mxene dispersion liquid, wherein the mass ratio of the graphene oxide to the Mxene is 1:0.5-2, and uniformly mixing the graphene oxide dispersion liquid and the Mxene dispersion liquid in an ultrasonic manner; and (3) filling the mixed dispersion liquid into a hydrothermal reaction kettle, reacting for 30-180min at the temperature of 60-120 ℃, and cleaning and drying to obtain the Mxene reinforced graphene.
In one embodiment, in the third step, the Mxene reinforced graphene is added into the elastic polymer monomer liquid, the ratio of the Mxene reinforced graphene to the elastic polymer monomer or the monomer polymer is 1:5-50, after the mixture is uniformly mixed, the monomer is polymerized by adding an initiator into the mixed liquid, and then the Mxene reinforced graphene elastic polymer film is obtained by suction filtration and drying at 100 ℃.
In one embodiment, the elastic polymer monomer liquid is one of polyurethane monomer liquid, PDMS monomer liquid, PVC monomer liquid or polyurethane solution, silicone resin solution and emulsion solution.
The invention further aims to provide a micro-sound sensing detector prepared according to the graphene acousto-optic signal conversion film based on the Mxene enhancement, wherein the graphene acousto-optic signal conversion film based on the Mxene enhancement has the thickness of 30-200um and the frequency response range of 50-1000Hz.
In one embodiment, the micro-acoustic sensing probe comprises: a sound intensity current characteristic spectrum and biological characteristic current signal tester and an underwater sonar detector.
Another object of the present invention is to provide a thin film piezoresistive sensor device based on Mxene enhanced graphene acousto-electric signal conversion thin film sensing performance test, the thin film piezoresistive sensor device comprising: and bonding conductive copper foils at two ends of the graphene acoustic-electric signal conversion film based on Mxene enhancement with the same size, connecting electrochemical workstations at two ends, bonding the graphene acoustic-electric signal conversion film to the surface of a commercial sound box, and testing acoustic sensing performance.
By combining all the technical schemes, the invention has the advantages and positive effects that:
according to the invention, single-layer or few-layer Mxene is used as a reinforcing phase, and is mixed with graphene oxide in a solution mode, and the Mxene reinforcing graphene is obtained through hydrothermal reaction. And mixing the Mxene reinforced graphene oxide with an elastic polymer monomer, and carrying out in-situ shrinkage polymerization on the elastic polymer monomer, and carrying out suction filtration to form a film to obtain the Mxene reinforced graphene elastic polymer film. The film has good elasticity, and the Mxene reinforced graphene conductive network distributed in the film can effectively convert sound wave vibration into an electric signal even under extremely fine sound vibration, so that an efficient ground sound/electric signal conversion effect is realized.
The novel micro-nano electronic material and device constructed from the micro-nano scale can effectively solve the problems existing in the background technology, for example, the appearance of novel two-dimensional material graphene and Mxene (Mxene material is a metal carbide and metal nitride material with a two-dimensional layered structure, and the appearance of the novel two-dimensional material is similar to potato chips with stacked chip pieces) can effectively solve the manufacturing problems of the micro-sound pickup. The extremely thin thickness results in a very small mass of the membrane and very small bending stiffness, and small changes in sound pressure can cause vibration of the suspended membrane. Since the extremely thin thickness results in a very small bending stiffness of the membrane, the sound pressure causes little resistance to out-of-plane bending vibration of the membrane. By detecting the vibration of the film, extremely weak sound signals can be captured and recorded. The overall vibration of the recording film reflects and counts weak sound pressure disturbances at the molecular level. Detecting vibration of the membrane generally becomes a simpler and more effective means of detecting faint audible information. The micro-sound pick-up manufactured by using the two-dimensional film can improve the recording accuracy of weak sound by many orders of magnitude.
The MXene reinforced graphene film constructed by the method has extremely thin thickness and bending rigidity, and the film supported by suspension can vibrate due to tiny sound pressure change. The enhancement of the Mxene on the graphene structure is utilized, and the two-dimensional conductive thin layer structure of the Mxene can not only improve the structural stability of the graphene, but also improve the sensitivity of the film to vibration signals. Compared with the acoustic-electric signal conversion film based on graphene or Mxene materials reported in the prior art, the acoustic-electric signal conversion film has better acoustic response frequency, shorter response time and higher sensitivity. Meanwhile, the manufacturing cost is greatly reduced, and the mass production is possible.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the disclosure and together with the description, serve to explain the principles of the disclosure;
fig. 1 is a flowchart of a preparation method of a graphene acousto-optic signal conversion film based on Mxene enhancement, which is provided by an embodiment of the invention;
fig. 2 is a diagram showing the effect of an electroacoustic signal conversion film placed on an acoustic test stand according to an embodiment of the present invention.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to the appended drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit or scope of the invention, which is therefore not limited to the specific embodiments disclosed below.
1. Explanation of the examples:
the embodiment of the invention provides a graphene acoustic-electric signal conversion film based on Mxene enhancement, which converts vibration acoustic signals into electric signals with multiple orders of magnitude by using a distributed Mxene enhanced graphene conductive network.
In the embodiment of the invention, the Mxene enhanced graphene conductive network is of a Mxene enhanced two-dimensional conductive thin layer structure.
The embodiment of the invention provides a preparation method of a graphene acousto-optic signal conversion film based on Mxene enhancement, which comprises the following steps:
s101, preparing a single-layer few-layer Mxene material;
s102, using a single-layer or less-layer Mxene material as a reinforcing phase, mixing the reinforcing phase with graphene oxide in a solution mode, and obtaining Mxene reinforced graphene through a hydrothermal reaction;
s103, mixing the Mxene reinforced graphene with an elastic polymer monomer, performing in-situ shrinkage polymerization on the elastic polymer monomer, and performing suction filtration to form a film to obtain the Mxene reinforced graphene elastic polymer film.
In step S101, the preparation of Mxene material includes: adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:10-40, the HCl concentration in the HCl solution is 9M & mol/L, and the stirring time is 20-120min;
ti is mixed with 3 AlC 2 Adding the powder into the mixed solution in batches and fully stirring for reaction; ti (Ti) 3 AlC 2 The proportion of the mixed solution is 1:10-100, wherein the reaction temperature is 20-60 ℃ and the reaction time is 12-48h;
after complete reaction, deionized water is added for washing until the pH value is 7; adding ethanol for cleaning, centrifuging at 10000r/min for 10min to remove supernatant, adding deionized water again, and centrifuging at 3500r/min for 3min to obtain MXene supernatant.
In step S102, the preparation of Mxene-enhanced graphene includes the following steps: mixing graphene oxide dispersion liquid and Mxene dispersion liquid, wherein the mass ratio of the graphene oxide to the Mxene is 1:0.5-2, and uniformly mixing the graphene oxide dispersion liquid and the Mxene dispersion liquid in an ultrasonic manner; and (3) filling the mixed dispersion liquid into a hydrothermal reaction kettle, reacting for 30-180min at the temperature of 60-120 ℃, and cleaning and drying to obtain the Mxene reinforced graphene.
In step S103, the Mxene reinforced graphene is added into elastic polymer monomer liquid, the ratio of the Mxene reinforced graphene to the elastic polymer monomer or the monomer polymer is 1:5-50, after the mixture is uniformly mixed, the monomer is polymerized by adding an initiator into the mixed liquid, and then the Mxene reinforced graphene elastic polymer film is obtained through suction filtration and drying at 100 ℃.
The film has good elasticity, and the Mxene reinforced graphene conductive network distributed in the film can effectively convert sound wave vibration into an electric signal even under extremely fine sound vibration, so that an efficient ground sound/electric signal conversion effect is realized.
Example 1
The preparation method of the graphene acousto-optic signal conversion film based on Mxene enhancement provided by the embodiment of the invention comprises the following steps:
s1, preparing a single-layer few-layer Mxene: using HCl/LiF solution for Ti 3 AlC 2 Etching and layering the powder to obtain MXene dispersion;
adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:10, the HCl concentration in the HCl solution is 9M (mol/L), and the stirring time is 120min;
then Ti is added 3 AlC 2 Adding the powder into the mixed solution in batches and fully stirring for reaction; ti (Ti) 3 AlC 2 The ratio of the powder to the mixed solution is 1:50, the reaction temperature is 50 ℃, and the reaction time is 48 hours;
after complete reaction, deionized water is added for repeated washing until the pH value is 7; and then adding ethanol for cleaning, centrifuging for 10min at 10000r/min to remove supernatant, adding deionized water again, and centrifuging for 3min at 3500r/min to obtain a few-layer MXene supernatant.
S2, preparing Mxene reinforced graphene: and mixing the graphene oxide dispersion liquid with the Mxene dispersion liquid to ensure that the mass ratio of the graphene oxide to the Mxene is 1:0.5, and uniformly mixing the graphene oxide and the Mxene in an ultrasonic mode. And then the mixed dispersion liquid is filled into a hydrothermal reaction kettle to react for 180min at the temperature of 120 ℃. And then cleaning and drying to obtain the Mxene reinforced graphene.
S3, preparing a composite film: and adding the Mxene reinforced graphene into elastic polymer monomer liquid, and obtaining the Mxene reinforced graphene and elastic polymer composite dispersion liquid through in-situ polymerization of the elastic polymer. And then the composite dispersion liquid is subjected to suction filtration and drying to obtain the graphene elastic polymer film based on Mxene enhancement, namely the graphene acousto-electric signal conversion film based on Mxene enhancement. The ratio of the MXene reinforced graphene to the elastic high polymer monomer or the monomer high polymer is 1:20, and the elastic high polymer monomer liquid is an organic silicon resin solution. Mixing uniformly. And (3) adding an initiator into the mixed solution to polymerize the monomer, and performing suction filtration and drying at 100 ℃ to obtain the Mxene reinforced graphene elastic polymer film.
And assembling the obtained Mxene reinforced graphene elastic polymer film into an acoustic sensor, and performing an acousto-optic signal test. As shown in fig. 2.
Example 2
The preparation method of the graphene acousto-optic signal conversion film based on Mxene enhancement provided by the embodiment of the invention comprises the following steps:
s1, preparing a single-layer few-layer Mxene: using HCl/LiF solution for Ti 3 AlC 2 Etching and layering the powder to obtain MXene dispersion;
adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:40, the HCl concentration in the HCl solution is 9M (mol/L), and the stirring time is 60min;
then Ti is added 3 AlC 2 Adding the powder into the mixed solution in batches and fully stirring for reaction; ti (Ti) 3 AlC 2 The ratio of the powder to the mixed solution is 1:10, the reaction temperature is 20 ℃ and the reaction time is 12 hours;
after complete reaction, deionized water is added for repeated washing until the pH value is 7; and then adding ethanol for cleaning, centrifuging for 10min at 10000r/min to remove supernatant, adding deionized water again, and centrifuging for 3min at 3500r/min to obtain a few-layer MXene supernatant.
S2, preparing Mxene reinforced graphene: and mixing the graphene oxide dispersion liquid with the Mxene dispersion liquid to ensure that the mass ratio of the graphene oxide to the Mxene is 1:1, and uniformly mixing the graphene oxide and the Mxene in an ultrasonic mode. And then the mixed dispersion liquid is filled into a hydrothermal reaction kettle to react for 120min at the temperature of 60 ℃. And then cleaning and drying to obtain the Mxene reinforced graphene.
S3, preparing a composite film: and adding the Mxene reinforced graphene into elastic polymer monomer liquid, and obtaining the Mxene reinforced graphene and elastic polymer composite dispersion liquid through in-situ polymerization of the elastic polymer. And then the composite dispersion liquid is subjected to suction filtration and drying to obtain the graphene elastic polymer film based on Mxene enhancement, namely the graphene acousto-electric signal conversion film based on Mxene enhancement. The ratio of the MXene reinforced graphene to the elastic high polymer monomer or the monomer high polymer is 1:5, and the elastic high polymer monomer liquid is polyurethane solution. Mixing uniformly. And (3) adding an initiator into the mixed solution to polymerize the monomer, and performing suction filtration and drying at 100 ℃ to obtain the Mxene reinforced graphene elastic polymer film.
And assembling the obtained Mxene reinforced graphene elastic polymer film into an acoustic sensor, and performing an acousto-optic signal test.
Example 3
The preparation method of the graphene acousto-optic signal conversion film based on Mxene enhancement provided by the embodiment of the invention comprises the following steps:
s1, preparing a single-layer few-layer Mxene: using HCl/LiF solution for Ti 3 AlC 2 Etching and layering the powder to obtain MXene dispersion;
adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:20, the HCl concentration in the HCl solution is 9M (mol/L), and the stirring time is 20min;
then Ti is added 3 AlC 2 Adding and mixing the powder in batchesStirring the solution fully for reaction; ti (Ti) 3 AlC 2 The ratio of the powder to the mixed solution is 1:100, the reaction temperature is 40 ℃ and the reaction time is 18 hours;
after complete reaction, deionized water is added for repeated washing until the pH value is 7; and then adding ethanol for cleaning, centrifuging for 10min at 10000r/min to remove supernatant, adding deionized water again, and centrifuging for 3min at 3500r/min to obtain a few-layer MXene supernatant.
S2, preparing Mxene reinforced graphene: and mixing the graphene oxide dispersion liquid with the Mxene dispersion liquid to ensure that the mass ratio of the graphene oxide to the Mxene is 1:2, and uniformly mixing the graphene oxide and the Mxene in an ultrasonic mode. And then the mixed dispersion liquid is filled into a hydrothermal reaction kettle to react for 30min at the temperature of 100 ℃. And then cleaning and drying to obtain the Mxene reinforced graphene.
S3, preparing a composite film: and adding the Mxene reinforced graphene into elastic polymer monomer liquid, and obtaining the Mxene reinforced graphene and elastic polymer composite dispersion liquid through in-situ polymerization of the elastic polymer. And then the composite dispersion liquid is subjected to suction filtration and drying to obtain the graphene elastic polymer film based on Mxene enhancement, namely the graphene acousto-electric signal conversion film based on Mxene enhancement. The ratio of the MXene reinforced graphene to the elastic polymer monomer or the monomer polymer is 1:50, and the elastic polymer monomer liquid is PDMS monomer solution. Mixing uniformly. And (3) adding an initiator into the mixed solution to polymerize the monomer, and performing suction filtration and drying at 100 ℃ to obtain the Mxene reinforced graphene elastic polymer film.
And assembling the obtained Mxene reinforced graphene elastic polymer film into an acoustic sensor, and performing an acousto-optic signal test.
Example 4
The preparation method of the graphene acousto-optic signal conversion film based on Mxene enhancement provided by the embodiment of the invention comprises the following steps:
s1, preparing a single-layer few-layer Mxene: using HCl/LiF solution for Ti 3 AlC 2 Etching and layering the powder to obtain MXene dispersion;
adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:30, the HCl concentration in the HCl solution is 9M (mol/L), and the stirring time is 100min;
then Ti is added 3 AlC 2 Adding the powder into the mixed solution in batches and fully stirring for reaction; ti (Ti) 3 AlC 2 The ratio of the powder to the mixed solution is 1:40, the reaction temperature is 25 ℃, and the reaction time is 36 hours;
after complete reaction, deionized water is added for repeated washing until the pH value is 7; and then adding ethanol for cleaning, centrifuging for 10min at 10000r/min to remove supernatant, adding deionized water again, and centrifuging for 3min at 3500r/min to obtain a few-layer MXene supernatant.
S2, preparing Mxene reinforced graphene: and mixing the graphene oxide dispersion liquid with the Mxene dispersion liquid to ensure that the mass ratio of the graphene oxide to the Mxene is 1:0.75, and uniformly mixing the graphene oxide and the Mxene in an ultrasonic mode. And then the mixed dispersion liquid is filled into a hydrothermal reaction kettle to react for 90min at the temperature of 80 ℃. And then cleaning and drying to obtain the Mxene reinforced graphene.
S3, preparing a composite film: and adding the Mxene reinforced graphene into elastic polymer monomer liquid, and obtaining the Mxene reinforced graphene and elastic polymer composite dispersion liquid through in-situ polymerization of the elastic polymer. And then the composite dispersion liquid is subjected to suction filtration and drying to obtain the graphene elastic polymer film based on Mxene enhancement, namely the graphene acousto-electric signal conversion film based on Mxene enhancement. The ratio of the MXene reinforced graphene to the elastic high polymer monomer or the monomer high polymer is 1:25, and the elastic high polymer monomer liquid is PVC monomer solution. Mixing uniformly. And (3) adding an initiator into the mixed solution to polymerize the monomer, and performing suction filtration and drying at 100 ℃ to obtain the Mxene reinforced graphene elastic polymer film.
And assembling the obtained Mxene reinforced graphene elastic polymer film into an acoustic sensor, and performing an acousto-optic signal test.
Example 5
The preparation method of the graphene acousto-optic signal conversion film based on Mxene enhancement provided by the embodiment of the invention comprises the following steps:
s1, preparing a single-layer few-layer Mxene: using HCl/LiF solution for Ti 3 AlC 2 Etching and layering the powder to obtain MXene dispersion;
adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:10, the HCl concentration in the HCl solution is 9M (mol/L), and the stirring time is 80min;
then Ti is added 3 AlC 2 Adding the powder into the mixed solution in batches and fully stirring for reaction; ti (Ti) 3 AlC 2 The ratio of the powder to the mixed solution is 1:80, the reaction temperature is 30 ℃, and the reaction time is 24 hours;
after complete reaction, deionized water is added for repeated washing until the pH value is 7; and then adding ethanol for cleaning, centrifuging for 10min at 10000r/min to remove supernatant, adding deionized water again, and centrifuging for 3min at 3500r/min to obtain a few-layer MXene supernatant.
S2, preparing Mxene reinforced graphene: and mixing the graphene oxide dispersion liquid with the Mxene dispersion liquid to ensure that the mass ratio of the graphene oxide to the Mxene is 1:1.5, and uniformly mixing the graphene oxide and the Mxene in an ultrasonic mode. And then the mixed dispersion liquid is filled into a hydrothermal reaction kettle to react for 150min at the temperature of 70 ℃. And then cleaning and drying to obtain the Mxene reinforced graphene.
S3, preparing a composite film: and adding the Mxene reinforced graphene into elastic polymer monomer liquid, and obtaining the Mxene reinforced graphene and elastic polymer composite dispersion liquid through in-situ polymerization of the elastic polymer. And then the composite dispersion liquid is subjected to suction filtration and drying to obtain the graphene elastic polymer film based on Mxene enhancement, namely the graphene acousto-electric signal conversion film based on Mxene enhancement. The ratio of the MXene reinforced graphene to the elastic high polymer monomer or the monomer high polymer is 1:40, and the elastic high polymer monomer liquid is an organosilicon solution. Mixing uniformly. And (3) adding an initiator into the mixed solution to polymerize the monomer, and performing suction filtration and drying at 100 ℃ to obtain the Mxene reinforced graphene elastic polymer film.
And assembling the obtained Mxene reinforced graphene elastic polymer film into an acoustic sensor, and performing an acousto-optic signal test.
Example 6
The preparation method of the graphene acousto-optic signal conversion film based on Mxene enhancement provided by the embodiment of the invention comprises the following steps:
s1, preparing a single-layer few-layer Mxene: using HCl/LiF solution for Ti 3 AlC 2 Etching and layering the powder to obtain MXene dispersion;
adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:10, the HCl concentration in the HCl solution is 9M (mol/L), and the stirring time is 120min;
then Ti is added 3 AlC 2 Adding the powder into the mixed solution in batches and fully stirring for reaction; ti (Ti) 3 AlC 2 The ratio of the powder to the mixed solution is 1:50, the reaction temperature is 50 ℃, and the reaction time is 48 hours;
after complete reaction, deionized water is added for repeated washing until the pH value is 7; and then adding ethanol for cleaning, centrifuging for 10min at 10000r/min to remove supernatant, adding deionized water again, and centrifuging for 3min at 3500r/min to obtain a few-layer MXene supernatant.
S2, preparing Mxene reinforced graphene: and mixing the graphene oxide dispersion liquid with the Mxene dispersion liquid to ensure that the mass ratio of the graphene oxide to the Mxene is 1:3, and uniformly mixing the graphene oxide and the Mxene in an ultrasonic mode. And then the mixed dispersion liquid is filled into a hydrothermal reaction kettle to react for 180min at the temperature of 120 ℃. And then cleaning and drying to obtain the Mxene reinforced graphene.
S3, preparing a composite film: and adding the Mxene reinforced graphene into elastic polymer monomer liquid, and obtaining the Mxene reinforced graphene and elastic polymer composite dispersion liquid through in-situ polymerization of the elastic polymer. And then the composite dispersion liquid is subjected to suction filtration and drying to obtain the graphene elastic polymer film based on Mxene enhancement, namely the graphene acousto-electric signal conversion film based on Mxene enhancement. The ratio of the MXene reinforced graphene to the elastic high polymer monomer or the monomer high polymer is 1:4, and the elastic high polymer monomer liquid is an organosilicon solution. Mixing uniformly. And (3) adding an initiator into the mixed solution to polymerize the monomer, and performing suction filtration and drying at 100 ℃ to obtain the Mxene reinforced graphene elastic polymer film.
And assembling the obtained Mxene reinforced graphene elastic polymer film into an acoustic sensor, and performing an acousto-optic signal test.
Example 7
The preparation method of the graphene acousto-optic signal conversion film based on Mxene enhancement provided by the embodiment of the invention comprises the following steps:
s1, preparing a single-layer few-layer Mxene: using HCl/LiF solution for Ti 3 AlC 2 Etching and layering the powder to obtain MXene dispersion;
adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:10, the HCl concentration in the HCl solution is 9M (mol/L), and the stirring time is 120min;
then Ti is added 3 AlC 2 Adding the powder into the mixed solution in batches and fully stirring for reaction; ti (Ti) 3 AlC 2 The ratio of the powder to the mixed solution is 1:50, the reaction temperature is 50 ℃, and the reaction time is 48 hours;
after complete reaction, deionized water is added for repeated washing until the pH value is 7; and then adding ethanol for cleaning, centrifuging for 10min at 10000r/min to remove supernatant, adding deionized water again, and centrifuging for 3min at 3500r/min to obtain a few-layer MXene supernatant.
S2, preparing Mxene reinforced graphene: and mixing the graphene oxide dispersion liquid with the Mxene dispersion liquid to ensure that the mass ratio of the graphene oxide to the Mxene is 1:0.3, and uniformly mixing the graphene oxide and the Mxene in an ultrasonic mode. And then the mixed dispersion liquid is filled into a hydrothermal reaction kettle to react for 180min at the temperature of 120 ℃. And then cleaning and drying to obtain the Mxene reinforced graphene.
S3, preparing a composite film: and adding the Mxene reinforced graphene into elastic polymer monomer liquid, and obtaining the Mxene reinforced graphene and elastic polymer composite dispersion liquid through in-situ polymerization of the elastic polymer. And then the composite dispersion liquid is subjected to suction filtration and drying to obtain the graphene elastic polymer film based on Mxene enhancement, namely the graphene acousto-electric signal conversion film based on Mxene enhancement. The ratio of the MXene reinforced graphene to the elastic high polymer monomer or the monomer high polymer is 1:60, and the elastic high polymer monomer liquid is an organosilicon solution. Mixing uniformly. And (3) adding an initiator into the mixed solution to polymerize the monomer, and performing suction filtration and drying at 100 ℃ to obtain the Mxene reinforced graphene elastic polymer film.
And assembling the obtained Mxene reinforced graphene elastic polymer film into an acoustic sensor, and performing an acousto-optic signal test.
Comparative example 1
The preparation method of the graphene acousto-optic signal conversion film based on Mxene enhancement comprises the following steps:
s1, preparing a single-layer few-layer Mxene: using HCl/LiF solution for Ti 3 AlC 2 Etching and layering the powder to obtain MXene dispersion;
adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:10, the HCl concentration in the HCl solution is 9M (mol/L), and the stirring time is 120min;
then Ti is added 3 AlC 2 Adding the powder into the mixed solution in batches and fully stirring for reaction; ti (Ti) 3 AlC 2 The ratio of the powder to the mixed solution is 1:50, the reaction temperature is 50 ℃, and the reaction time is 48 hours;
after complete reaction, deionized water is added for repeated washing until the pH value is 7; and then adding ethanol for cleaning, centrifuging for 10min at 10000r/min to remove supernatant, adding deionized water again, and centrifuging for 3min at 3500r/min to obtain a few-layer MXene supernatant.
S2, preparing a composite film: and adding the Mxene into elastic polymer monomer liquid, and obtaining the Mxene and elastic polymer composite dispersion liquid through in-situ polymerization of the elastic polymer. And then the composite dispersion liquid is subjected to suction filtration and drying to obtain an elastic polymer film based on Mxene, namely an acoustic-electric signal conversion film based on Mxene. Wherein the ratio of MXene to elastic polymer monomer or monomer polymer is 1:60, and the elastic polymer monomer liquid is organosilicon solution. Mixing uniformly. And (3) adding an initiator into the mixed solution to polymerize the monomer, and then carrying out suction filtration and drying at 100 ℃ to obtain the Mxene elastic polymer film.
And assembling the obtained Mxene elastic polymer film into an acoustic sensor, and testing an acousto-electric signal.
Comparative example 2
S1, loading the graphene oxide dispersion liquid into a hydrothermal reaction kettle, and reacting for 180min at the temperature of 120 ℃. And then cleaning and drying to obtain the graphene.
S2, preparing a composite film: and adding graphene into elastic polymer monomer liquid, and obtaining graphene and elastic polymer composite dispersion liquid through in-situ polymerization of elastic polymers. And then the composite dispersion liquid is subjected to suction filtration and drying to obtain a graphene elastic polymer film, namely a graphene acousto-electric signal conversion film. The ratio of the graphene to the elastic high molecular monomer or the monomer high polymer is 1:60, and the elastic high molecular monomer liquid is an organosilicon solution. Mixing uniformly. And adding an initiator into the mixed solution to polymerize the monomer, and performing suction filtration and drying at 100 ℃ to obtain the graphene elastic polymer film.
And assembling the graphene elastic polymer film into an acoustic sensor, and testing an acousto-electric signal.
Comparative example 1 is an MXene elastic polymer film and an acoustic sensor prepared using MXene, and comparative example 2 is a graphene elastic polymer film and an acoustic sensor prepared using graphene.
Performance test method
The performance test method for the embodiment of the invention comprises the following steps: bonding conductive copper foils on two ends of a film with the same size, connecting the two ends with electrochemical workstations, bonding the film to the surface of a commercial sound box, and testing sound sensing performance; and simultaneously, a tensile tester is used for testing the tensile strength and the tensile elongation of the film.
The test data for the examples and comparative examples are as follows:
from examples 1-5, examples 6-7, comparative examples. The MXene reinforced graphene acousto-electric signal conversion film provided by the invention has good mechanical strength and elongation, and can meet the requirement of converting acoustic sampling vibration into an electric signal. Meanwhile, the method has good response frequency, response time and sensitivity.
While the invention has been described with respect to what is presently considered to be the most practical and preferred embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but on the contrary, is intended to cover various modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (10)
1. The graphene acousto-electric signal conversion film based on Mxene enhancement is characterized in that the film converts vibration acoustic signals into electric signals of multiple orders of magnitude by using a distributed Mxene enhancement graphene conductive network.
2. The graphene acousto-electric signal conversion film based on Mxene enhancement according to claim 1, characterized in that the Mxene enhanced graphene conductive network is an Mxene enhanced two-dimensional conductive thin layer structure.
3. A method for preparing the graphene acousto-electric signal conversion film based on Mxene enhancement according to any one of claims 1 or 2, comprising:
step one, preparing a single-layer few-layer Mxene material;
step two, using an Mxene material as a reinforcing phase, mixing the reinforcing phase with graphene oxide in a solution mode, and obtaining the Mxene reinforced graphene through a hydrothermal reaction;
and thirdly, mixing the Mxene reinforced graphene with an elastic polymer monomer, and performing in-situ shrinkage polymerization on the elastic polymer monomer, and performing suction filtration to form a film to obtain the Mxene reinforced graphene elastic polymer film.
4. A method of preparing as claimed in claim 3, wherein in step one, the preparation of Mxene material comprises:
adding LiF powder into HCl solution, stirring and fully dissolving; the mass ratio of LiF powder to HCl solution is 1:10-40, the HCl concentration in the HCl solution is 9M & mol/L, and the stirring time is 20-120min;
ti is mixed with 3 AlC 2 Adding the powder into the mixed solution in batches and fully stirring for reaction; ti (Ti) 3 AlC 2 The ratio of the powder to the mixed solution is 1:10-100, wherein the reaction temperature is 20-60 ℃ and the reaction time is 12-48h;
after complete reaction, deionized water is added for washing until the pH value is 7; adding ethanol for cleaning, centrifuging at 10000r/min for 10min to remove supernatant, adding deionized water again, and centrifuging at 3500r/min for 3min to obtain MXene supernatant.
5. A method of preparing as claimed in claim 3, wherein in step two, the preparation of Mxene enhanced graphene comprises the steps of:
mixing graphene oxide dispersion liquid and Mxene dispersion liquid, wherein the mass ratio of the graphene oxide to the Mxene is 1:0.5-2, and uniformly mixing the graphene oxide dispersion liquid and the Mxene dispersion liquid in an ultrasonic manner; and (3) filling the mixed dispersion liquid into a hydrothermal reaction kettle, reacting for 30-180min at the temperature of 60-120 ℃, and cleaning and drying to obtain the Mxene reinforced graphene.
6. The preparation method of claim 3, wherein in the third step, mxene reinforced graphene is added into elastic polymer monomer liquid, the ratio of Mxene reinforced graphene to elastic polymer monomer or monomer polymer is 1:5-50, after mixing uniformly, the monomer is polymerized by adding initiator into the mixed liquid, and then suction filtration and 100 ℃ drying are carried out to obtain Mxene reinforced graphene elastic polymer film.
7. The method according to claim 6, wherein the elastic polymer monomer liquid is one of polyurethane monomer liquid, PDMS monomer liquid, PVC monomer liquid, polyurethane solution, silicone resin solution, and latex solution.
8. A micro-acoustic sensing detector prepared based on an Mxene enhanced graphene acoustic-electric signal conversion film according to any one of claims 1-2, characterized in that the Mxene enhanced graphene acoustic-electric signal conversion film has a thickness of 30-200um and a frequency response range of 50-1000Hz.
9. The micro-acoustic sensing probe of claim 8, wherein the micro-acoustic sensing probe comprises: a sound intensity current characteristic spectrum and biological characteristic current signal tester and an underwater sonar detector.
10. A thin film piezoresistive sensor device for Mxene enhanced graphene acoustic-electric signal conversion thin film sensing performance test according to any one of claims 1-2, characterized in that said thin film piezoresistive sensor device comprises: and bonding conductive copper foils at two ends of the graphene acoustic-electric signal conversion film based on Mxene enhancement, connecting electrochemical workstations at two ends, bonding to the surface of a commercial sound box, and testing acoustic sensing performance.
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