CN113193107A - Monoatomic piezoelectric material and preparation method and application thereof - Google Patents
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- H10N30/03—Assembling devices that include piezoelectric or electrostrictive parts
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a monatomic piezoelectric material and a preparation method and application thereof. The preparation method comprises the following steps: at least carrying out hydrothermal reaction on the piezoelectric material and a metal monatomic source at 140-180 ℃ to obtain the monatomic piezoelectric material. The monatomic piezoelectric material prepared by the method can change the surface potential of the carrier through the chemical bonding action of the metal monatomic and the surface of the piezoelectric material based on the coordination regulation principle between the monatomic and the carrier, and can obviously influence the piezoelectric performance of the substrate material, and the piezoelectric performance of the monatomic piezoelectric material prepared by the method is improved by nearly 10 times compared with that of the traditional piezoelectric material; the preparation method provided by the invention is based on the micro-chemical action of the heterogeneous interface of the material, has universality and provides a brand-new technical approach for improving the performance of the piezoelectric material.
Description
Technical Field
The invention belongs to the technical field of new energy materials, and particularly relates to a monatomic piezoelectric material and a preparation method and application thereof.
Background
The piezoelectric effect indicates that when some materials are subjected to external force along a certain direction, the material structure is subjected to microscopic deformation, a polarization phenomenon is generated in the material structure, and positive and negative opposite charges appear on two opposite surfaces of the material structure. When the external force is removed, it returns to its uncharged state, a phenomenon known as the piezoelectric effect. When the direction of the force changes, the polarity of the charge changes. For this reason, piezoelectric devices have become ubiquitous, such as quartz oscillators, microbalances with sub-atomic resolution. For example, Boron Nitride (BN) is a typical piezoelectric material, has high chemical stability and thermal stability, can be applied as a piezoelectric thin film in surface acoustic wave devices, and in recent years, a major research focus of high frequency Surface Acoustic Wave (SAW) devices is a substrate material having high acoustic velocity and excellent piezoelectric properties. Compared with the traditional low sound velocity materials such as ZnO and LiNbO3Compared with the materials, the BN piezoelectric film phase velocity is superior to the materials, so that the SAW device can reach higher frequency, and the high-frequency SAW device with low frequency dispersion and good frequency temperature coefficient can be realized. But the piezoelectric property of BN is relative to that of the traditional piezoelectric materials of ZnO and LiNbO3In terms of performance, the performance is poor. At present, two methods for improving the BN piezoelectric performance can be adopted, wherein the first method is to thin the number of BN layers to obtain a few or even single-layer BN nanosheets, and research shows that the piezoelectric performance can be improved when the number of BN layers is reduced, but the method has complexity and instability; another way is to improve the piezoelectric performance by mixing BN with other piezoelectric materials, but this method has insignificant improvement effect and unstable performance. Therefore, it is important to find an effective method for improving the BN piezoelectric property and the traditional piezoelectric material.
Disclosure of Invention
The invention mainly aims to provide a monatomic piezoelectric material, and a preparation method and application thereof, so as to overcome the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of a monatomic piezoelectric material, which comprises the following steps:
at least carrying out hydrothermal reaction on the piezoelectric material and a metal monatomic source at 140-180 ℃ to obtain the monatomic piezoelectric material.
Further, the piezoelectric material comprises h-BN and MoS2、SnS2、MoSe2、SnO2、WS2、CrTe2Any one or a combination of two or more of them, and is not limited thereto.
Further, the metal monatomic source includes a metal inorganic substance and/or a metal organic substance.
Further, the metal monatomic source includes W (CO)6、W(CO)4、Cr(CO)6、Ni(CO)4、Mo(CO)6、Na2WO4Any one or a combination of two or more of them, and is not limited thereto.
The embodiment of the invention also provides the monatomic piezoelectric material prepared by the method.
The embodiment of the invention also provides application of the monatomic piezoelectric material in preparation of piezoelectric devices.
The embodiment of the invention also provides a preparation method of the piezoelectric device, which comprises the following steps:
preparing the monatomic piezoelectric material by adopting the method;
and uniformly mixing the monatomic piezoelectric material, the packaging material and the curing agent, then applying the obtained mixture to the surface of a conductive substrate, and forming the piezoelectric device through assembly.
The embodiment of the invention also provides a piezoelectric device prepared by the method, and the piezoelectric device comprises a first conductive glass layer, a piezoelectric material layer and a second conductive glass layer which are sequentially arranged along a set direction, wherein the piezoelectric material layer is formed by solidifying the monatomic piezoelectric material and the packaging material.
The embodiment of the invention also provides a method for improving the performance of the piezoelectric material, which comprises the following steps: at least enabling the piezoelectric material and a metal monatomic source to carry out hydrothermal reaction at 140-180 ℃, so that the piezoelectric material loads metal monatomics.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method takes a piezoelectric material as a carrier, takes a metal inorganic substance or a metal organic substance as a metal monatomic source, synthesizes the monatomic piezoelectric material by a hydrothermal high-temperature high-pressure method, and improves the piezoelectric performance of the material by coordination of the metal monatomic and atoms on the surface of the piezoelectric material; in a piezoelectric performance test experiment, compared with an original piezoelectric material, the piezoelectric performance of the monatomic piezoelectric material is improved by nearly 10 times, and surface potential is changed by coordination of monatomic metal and atoms on the surface of a carrier, so that the piezoelectric performance of the piezoelectric material is improved;
(2) the preparation method of the monatomic piezoelectric material provided by the invention has universality, and the selected carrier material can be expanded to SnS2、MoS2、SnO2、WS2、MoSe2、CrTe2And the selected metal monatomic source can be metal inorganic matters or metal organic matters such as Co, Pt, Mo, Ni, Pd, Rh and the like, and the method can provide a new research idea for the preparation of the monatomic material and the exploration of a piezoelectric mechanism.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a structural view of a piezoelectric device produced in example 1 of the present invention;
FIG. 2 is a graph showing piezoelectric signals of different devices under the same pressure in the piezoelectric devices prepared in example 1 of the present invention and comparative examples 1 to 2;
FIG. 3 is a spherical aberration electron micrograph of W monoatomic supported h-BN (W-BN) as a final product in example 1 of the present invention.
Detailed Description
In view of the defects of the prior art, the inventor of the present invention has long studied and largely practiced to propose the technical solution of the present invention, which will be clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
One aspect of an embodiment of the present invention provides a method for preparing a monatomic piezoelectric material, including:
at least carrying out hydrothermal reaction on the piezoelectric material and a metal monatomic source at 140-180 ℃ to obtain the monatomic piezoelectric material.
In some more specific embodiments, the piezoelectric material comprises h-BN, MoS2、SnS2、MoSe2、SnO2、WS2、CrTe2Any one or a combination of two or more of them, and is not limited thereto.
Further, the piezoelectric material is a two-dimensional piezoelectric material.
Further, the metal monatomic source includes a metal inorganic substance and/or a metal organic substance, and is not limited thereto.
Further, the metal forming the metal inorganic substance and/or the metal organic substance includes any one or a combination of two or more of W, Cr, Co, Pt, Mo, Ni, Pd, Rh, and is not limited thereto.
Further, the metal organic includes a metal carbonyl organic complex, and is not limited thereto.
Further, the metal monatomic source includes W (CO)6、W(CO)4、Cr(CO)6、Ni(CO)4、Mo(CO)6、Na2WO4Any one or a combination of two or more of them; particularly preferred is W (CO)6。
In some more specific embodiments, the preparation method comprises: and mixing the piezoelectric material with a metal monatomic source and a solvent, and then carrying out the hydrothermal reaction for 2-6 h.
Further, mixing a piezoelectric material, a metal monatomic source and a solvent to form a hydrothermal reaction system, and then heating the hydrothermal reaction system to 140-180 ℃ at a heating rate of 5-10 ℃/min and carrying out hydrothermal reaction to obtain the monatomic piezoelectric material.
Further, the solvent includes a mixed solvent of toluene and oleylamine, and is not limited thereto.
Further, the temperature increase rate is preferably any one of 5 ℃/min, 6 ℃/min, 7 ℃/min, 8 ℃/min, and 9 ℃/min.
Further, the temperature of the hydrothermal reaction is any one of 140 ℃, 150 ℃, 160 ℃, 170 ℃ and 180 ℃.
Further, the hydrothermal reaction time is any one of 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h and 6 h.
In some more specific embodiments, the preparation method further comprises: and after the hydrothermal reaction is finished, washing, separating and drying the obtained mixture.
Further, the washing solvent used in the washing treatment includes any one or a combination of two or more of ethanol, n-hexane, cyclohexane, ethanol, and chloroform, and is not limited thereto.
Furthermore, the drying treatment temperature is 40-80 ℃, and the drying treatment time is 6-10 h.
Further, the temperature of the drying treatment is any one of 40 ℃, 45 ℃, 50 ℃, 55 ℃, 65 ℃, 70 ℃, 75 ℃ and 80 ℃.
Another aspect of an embodiment of the present invention also provides a monatomic piezoelectric material produced by the foregoing method.
Furthermore, the monatomic piezoelectric material comprises a piezoelectric material serving as a carrier and a metal monatomic loaded on the surface of the carrier, wherein the metal monatomic is loaded on the surface of the carrier through chemical bonding with atoms on the surface of the carrier.
Furthermore, the content of metal single atoms in the single-atom piezoelectric material is 1.5-2.5 wt%.
Another aspect of the embodiments of the present invention also provides a use of the aforementioned monatomic piezoelectric material in the preparation of a piezoelectric device.
Another aspect of an embodiment of the present invention also provides a method for manufacturing a piezoelectric device, including:
preparing the monatomic piezoelectric material by adopting the method;
and uniformly mixing the monatomic piezoelectric material, the packaging material and the curing agent, then applying the obtained mixture to the surface of a conductive substrate, and forming the piezoelectric device through assembly.
In some more specific embodiments, the preparation method specifically comprises:
mixing the monatomic piezoelectric material with a dispersing agent to form monatomic piezoelectric material dispersion liquid, adding a packaging material, uniformly mixing, and then drying to obtain a mixture of the monatomic piezoelectric material and the packaging material;
and uniformly mixing the mixture of the monatomic piezoelectric material and the encapsulating material with a curing agent, and then applying the obtained mixture to a conductive surface of a conductive substrate and forming the piezoelectric device by assembly.
Further, the encapsulation material includes polydimethylsiloxane, and is not limited thereto.
Further, the dispersant includes ethanol and/or acetone, and is not limited thereto.
Further, the curing agent includes hydrogen-containing silicone oil, and is not limited thereto.
Further, the curing agent includes dimethyl silicone oil, and is not limited thereto.
Further, the conductive substrate includes a conductive glass, and is not limited thereto.
Furthermore, the conductive glass is single-sided conductive glass.
Further, the single-sided conductive glass includes any one or a combination of two or more of ITO conductive glass, FTO conductive glass, and PET-ITO conductive film, which are coated with indium tin oxide on a single side, and is not limited thereto.
Further, the preparation method comprises the following steps: the obtained mixture is applied to the conductive surface of the conductive glass by spin coating and/or spray coating and assembled to form the piezoelectric device.
Further, the preparation method comprises the following steps: and spin-coating the obtained mixture on the conductive surface of the conductive glass at a spin-coating speed of 600-1200 rpm, and assembling to form the piezoelectric device.
Further, the spin-coating rotation speed is any one of 600rpm, 700rpm, 800rpm, 900rpm, 1100rpm, 1200 rpm.
Further, the mass ratio of the packaging material to the curing agent is 10-20: 1.
Further, the mass ratio of the packaging material to the curing agent is any one of 10: 1, 12: 1, 14: 1, 16: 1, 18: 1 and 20: 1.
In some more specific embodiments, the method of manufacturing a piezoelectric device specifically includes:
and mixing the monatomic piezoelectric material with PDMS, then adding a curing agent for stirring, and finally performing spin coating to distribute the mixture on ITO conductive glass and assembling the ITO conductive glass into a device.
Wherein, when the PDMS is cured, the curing ratio is 10: 1, and the PDMS is always contacted with the conductive surface of the ITO.
The test of the piezoelectric performance of the invention is to apply pressure to the device circularly and constantly by equipment such as a stepper and/or a circular press, and then collect piezoelectric signals by electronic equipment such as a Tak oscilloscope, a voltmeter, an electrochemical workstation and the like.
Another aspect of an embodiment of the present invention also provides a piezoelectric device prepared by the foregoing method, including a first conductive glass layer, a piezoelectric material layer, and a second conductive glass layer sequentially arranged along a set direction, the piezoelectric material layer being formed by curing the monatomic piezoelectric material and the encapsulating material.
Furthermore, the first conductive glass layer and the second conductive glass layer are both single-sided conductive glass.
Further, the single-sided conductive glass includes any one or a combination of two or more of ITO conductive glass, FTO conductive glass, and PET-ITO conductive film, which are coated with indium tin oxide on a single side, and is not limited thereto.
Furthermore, the conductive surfaces of the first conductive glass layer and the second conductive glass layer are in contact with the piezoelectric material layer.
Furthermore, the thickness of the piezoelectric material layer is 0.4-0.6 mm, and preferably 0.5 mm.
In some more specific embodiments, the method for preparing the monatomic piezoelectric material specifically includes:
with h-BN nanoplate and W (CO)6As a raw material, a monatomic W-supported h-BN two-dimensional material (W-BN) was successfully prepared by a hydrothermal method of a high-temperature high-pressure reaction maintained at 150 ℃ for 4 hours.
Correspondingly, the preparation method of the piezoelectric device specifically comprises the following steps:
the W-BN, PDMS and ITO conductive glass are assembled into a device, piezoelectric performance test and piezoelectric signal collection are carried out through a stepper and an oscilloscope, and piezoelectric signals of the piezoelectric material loaded by the single atom are improved by about 10 times compared with those of the original substrate material.
The invention also provides a method for improving the performance of the piezoelectric material, which comprises the following steps: at least enabling the piezoelectric material and a metal monatomic source to carry out hydrothermal reaction at 140-180 ℃, so that the piezoelectric material loads metal monatomics.
In some more specific embodiments, the hydrothermal reaction is performed after mixing the piezoelectric material with a metal monatomic source and a solvent.
Further, mixing a piezoelectric material, a metal monatomic source and a solvent to form a hydrothermal reaction system, and then heating the hydrothermal reaction system to 140-180 ℃ at a heating rate of 5-10 ℃/min and carrying out the hydrothermal reaction;
in some more specific embodiments, the piezoelectric material comprises h-BN, MoS2、SnS2、MoSe2、SnO2、WS2、CrTe2Any one or a combination of two or more of them, and is not limited thereto.
Further, the piezoelectric material is a two-dimensional piezoelectric material.
In some more specific embodiments, the source of metal monatomic includes, but is not limited to, a metallomineral and/or a metalloorganic.
Further, the metal forming the metal inorganic substance and/or the metal organic substance includes any one or a combination of two or more of W, Cr, Co, Pt, Mo, Ni, Pd, Rh, and is not limited thereto.
Further, the metal organic includes a metal carbonyl organic complex, and is not limited thereto.
Further, the metal monatomic source includes W (CO)6、W(CO)4、Cr(CO)6、Ni(CO)4、Mo(CO)6、Na2WO4Any one or a combination of two or more thereof, particularly preferably W (CO)6。
Further, the solvent includes a mixed solvent of toluene and oleylamine, and is not limited thereto.
In some more specific embodiments, after the hydrothermal reaction is completed, the obtained mixture is washed, separated, and dried.
Further, the washing solvent used in the washing treatment includes any one or a combination of two or more of ethanol, n-hexane, cyclohexane, ethanol, and chloroform, and is not limited thereto.
Furthermore, the drying treatment temperature is 40-80 ℃, and the drying treatment time is 6-10 h.
The invention discloses a method for improving the piezoelectric performance of a material, and demonstrates an efficient monatomic piezoelectric material. The metal monatomic is coordinated with atoms on the surface of the piezoelectric material and combined, so that the potential on the surface of the piezoelectric material is generated, and the polarizability is increased under the condition of mechanical external force, and the performance of the piezoelectric material is improved by about 10 times by taking the monatomic loaded h-BN nanosheet as an example. The method can provide a novel research method for the piezoelectric material to improve the piezoelectric performance and the mechanism research.
The piezoelectric effect is generated microscopically because the material structure generates microscopic deformation, the polarization phenomenon can be generated in the material structure, and the surface potential changes.
The technical solutions of the present invention are further described in detail below with reference to several preferred embodiments and the accompanying drawings, which are implemented on the premise of the technical solutions of the present invention, and a detailed implementation manner and a specific operation process are provided, but the scope of the present invention is not limited to the following embodiments.
The experimental materials used in the examples used below were all available from conventional biochemical reagents companies, unless otherwise specified.
Example 1
Weighing 50mg of h-BN, 20mg of W (CO)6Placing the mixture into a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, sealing the reaction kettle, heating to 150 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 4 hours, naturally cooling a product in the reaction kettle, collecting the product by a suction filtration method, and drying in a vacuum oven at 60 ℃ for 10 hours to obtain the final product W monatomic loaded h-BN (recorded as W-BN). The obtained W-BN can see the existence of single atoms through a spherical aberration electron microscope picture, and the successful load of the single atoms is shown in figure 3, and the metal single atoms are shown as white dots in the picture.
Weighing a certain amount of final product W-BN, ultrasonically dispersing in ethanol, adding 1g of PDMS into the ethanol and W-BN mixed solution, stirring for 0.5h on a magnetic stirrer to ensure that the W-BN is uniformly dispersed in the PDMS, then putting the mixture into a vacuum oven, drying for 6h at 80 ℃ to ensure that the ethanol is completely evaporated, then taking out the mixture, then adding 0.1g of dimethicone into the PDMS mixed with the W-BN and uniformly stirring, then uniformly spin-coating the mixture on a conductive surface of ITO conductive glass by a spin-coating method, then covering a layer of ITO conductive glass on the conductive surface to collect charges, finally applying pressure to a device by a stepper, and collecting piezoelectric signals by an oscilloscope.
Example 2
50mg of h-BN, 40mg of W (CO)6Placing the mixture into a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, sealing the reaction kettle, heating to 150 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 4 hours, naturally cooling a product in the reaction kettle, collecting the product by a suction filtration method, and drying in a vacuum oven at 60 ℃ for 10 hours to obtain the final product W monatomic loaded h-BN (W-BN). Weighing a certain amount of final product W-BN, ultrasonically dispersing in ethanol, adding 1g of PDMS into the ethanol and W-BN mixed solution, stirring for 0.5h on a magnetic stirrer to ensure that the W-BN is uniformly dispersed in the PDMS, then putting the mixture into a vacuum oven, drying for 6h at 80 ℃ to ensure that the ethanol is completely evaporated, then taking out the mixture, then adding 0.1g of dimethicone into the PDMS mixed with the W-BN and uniformly stirring, then uniformly spin-coating the mixture on a conductive surface of ITO conductive glass by a spin-coating method, then covering a layer of ITO conductive glass on the conductive surface to collect charges, finally applying pressure to a device by a stepper, and collecting piezoelectric signals by an oscilloscope.
Example 3
50mg of h-BN, 60mg of W (CO)6Placing the mixture into a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, sealing the reaction kettle, heating to 150 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 4 hours, naturally cooling a product in the reaction kettle, collecting the product by a suction filtration method, and drying in a vacuum oven at 60 ℃ for 10 hours to obtain the final product W monatomic loaded h-BN (W-BN). Weighing a certain amount of final product W-BN, ultrasonically dispersing in ethanol, and adding 1g of the final product W-BN into the ethanol and W-BN mixed solutionPDMS and stirring on a magnetic stirrer for 0.5h to ensure that W-BN is uniformly dispersed in PDMS, then putting the mixture into a vacuum oven, drying for 6h at 80 ℃ to ensure that ethanol is completely evaporated, then taking out the mixture, then adding 0.1g of dimethyl silicone oil into the PDMS mixed with W-BN and uniformly stirring, then uniformly spin-coating the mixture on the conductive surface of ITO conductive glass by a spin coating method, then covering a layer of ITO conductive glass on the upper layer of the mixture to collect charges, finally applying pressure on the device by a stepper, and collecting piezoelectric signals by an oscilloscope.
Example 4
Weighing 50mg of h-BN, 80mg of W (CO)6Placing the mixture into a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, sealing the reaction kettle, heating to 150 ℃ at the heating rate of 10 ℃/min, keeping the temperature for 4 hours, naturally cooling a product in the reaction kettle, collecting the product by a suction filtration method, and drying in a vacuum oven at 60 ℃ for 10 hours to obtain the final product W monatomic loaded h-BN (W-BN). Weighing a certain amount of final product W-BN, ultrasonically dispersing in ethanol, adding 1g of PDMS into the ethanol and W-BN mixed solution, stirring for 0.5h on a magnetic stirrer to ensure that the W-BN is uniformly dispersed in the PDMS, then putting the mixture into a vacuum oven, drying for 6h at 80 ℃ to ensure that the ethanol is completely evaporated, then taking out the mixture, then adding 0.1g of dimethicone into the PDMS mixed with the W-BN and uniformly stirring, then uniformly spin-coating the mixture on a conductive surface of ITO conductive glass by a spin-coating method, then covering a layer of ITO conductive glass on the conductive surface to collect charges, finally applying pressure to a device by a stepper, and collecting piezoelectric signals by an oscilloscope.
Example 5
Weighing 50mg of h-BN, 100mg of W (CO)6Placing in a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, sealing the reaction kettle, heating to 150 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 4h, and introducing after the product in the reaction kettle is naturally cooledAnd collecting the product by a suction filtration method, and drying the product in a vacuum oven at 60 ℃ for 10h to obtain the final product W monatomic loaded h-BN (W-BN). Weighing a certain amount of final product W-BN, ultrasonically dispersing in ethanol, adding 1g of PDMS into the ethanol and W-BN mixed solution, stirring for 0.5h on a magnetic stirrer to ensure that the W-BN is uniformly dispersed in the PDMS, then putting the mixture into a vacuum oven, drying for 6h at 80 ℃ to ensure that the ethanol is completely evaporated, then taking out the mixture, then adding 0.1g of dimethicone into the PDMS mixed with the W-BN and uniformly stirring, then uniformly spin-coating the mixture on a conductive surface of ITO conductive glass by a spin-coating method, then covering a layer of ITO conductive glass on the conductive surface to collect charges to form a piezoelectric device (shown in figure 1), finally applying pressure to the device by a stepper, and collecting piezoelectric signals by an oscilloscope. A piezoelectric performance chart of the piezoelectric device prepared in this example under a pressure of 18N is shown in fig. 2.
Example 6
50mg of MoS was weighed250mg of Ni (CO)4Placing the mixture into a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, sealing the reaction kettle, heating to 150 ℃ at a heating rate of 5 ℃/min, keeping the temperature for 4 hours, naturally cooling a product in the reaction kettle, collecting the product by a suction filtration method, and drying in a vacuum oven at 40 ℃ for 10 hours to obtain the final product of the Ni monatomic supported MoS2(Ni-MoS2). Weighing a certain amount of final product Ni-MoS2Ultrasonically dispersing in ethanol, and adding into the ethanol and Ni-MoS21g PDMS was added to the mixed solution and stirred on a magnetic stirrer for 0.5h, ensuring Ni-MoS2Uniformly dispersed in PDMS, then the mixture was placed in a vacuum oven and dried at 80 ℃ for 6h to ensure that the ethanol was completely evaporated, then it was taken out, and then Ni-MoS was added to the mixture2Adding 0.1g of dimethyl silicone oil into PDMS, stirring uniformly, uniformly spin-coating the mixture on the conductive surface of ITO conductive glass by a spin-coating method, and covering a layer of ITO conductive glass on the conductive surfaceAnd collecting electric charges, finally applying pressure to the device through a stepper, and collecting piezoelectric signals through an oscilloscope.
Example 7
50mg of MoS was weighed2100mg of Ni (CO)4Placing the mixture into a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, sealing the reaction kettle, heating to 150 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 4 hours, naturally cooling a product in the reaction kettle, collecting the product by a suction filtration method, and drying in a vacuum oven at 80 ℃ for 6 hours to obtain a final product of Ni monatomic-loaded MoS2(Ni-MoS2). Weighing a certain amount of final product Ni-MoS2Ultrasonically dispersing in ethanol, and adding into the ethanol and Ni-MoS21g PDMS was added to the mixed solution and stirred on a magnetic stirrer for 0.5h, ensuring Ni-MoS2Uniformly dispersed in PDMS, then the mixture was placed in a vacuum oven and dried at 80 ℃ for 6h to ensure that the ethanol was completely evaporated, then it was taken out, and then Ni-MoS was added to the mixture2Adding 0.1g of dimethyl silicone oil into PDMS, stirring uniformly, uniformly spin-coating the mixture on the conductive surface of ITO conductive glass by a spin-coating method, covering a layer of ITO conductive glass on the upper layer of the mixture to collect charges, applying pressure to the device by a stepper, and collecting piezoelectric signals by an oscilloscope.
Example 8
50mg of SnS is weighed250mg of Mo (CO)4Placing the mixture into a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, sealing the reaction kettle, heating to 150 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 4 hours, naturally cooling a product in the reaction kettle, collecting the product by a suction filtration method, and drying in a vacuum oven at 60 ℃ for 8 hours to obtain a final product Mo monatomic-loaded SnS2(Mo-SnS2). Weighing a certain amount of final product Mo-SnS2Ultrasonically dispersing in ethanol, and adding into the ethanol and Mo-SnS21g of PDM was added to the mixed solutionS is stirred for 0.5h on a magnetic stirrer, and Mo-SnS is ensured2Uniformly dispersed in PDMS, then the mixture was placed in a vacuum oven and dried at 80 ℃ for 6h to ensure complete evaporation of ethanol, then it was removed and Mo-SnS was added to the mixture2Adding 0.1g of dimethyl silicone oil into PDMS, stirring uniformly, uniformly spin-coating the mixture on the conductive surface of ITO conductive glass by a spin-coating method, covering a layer of ITO conductive glass on the upper layer of the mixture to collect charges, applying pressure to the device by a stepper, and collecting piezoelectric signals by an oscilloscope.
Example 9
50mg of SnS is weighed2100mg of Mo (CO)4Placing the mixture into a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, sealing the reaction kettle, heating to 150 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 4 hours, naturally cooling a product in the reaction kettle, collecting the product by a suction filtration method, and drying in a vacuum oven at 60 ℃ for 10 hours to obtain a final product Mo monatomic-loaded SnS2(Mo-SnS2). Weighing a certain amount of final product Mo-SnS2Ultrasonically dispersing in ethanol, and adding into the ethanol and Mo-SnS21g PDMS was added to the mixed solution and stirred on a magnetic stirrer for 0.5h, ensuring that Mo-SnS2Uniformly dispersed in PDMS, then the mixture was placed in a vacuum oven and dried at 80 ℃ for 6h to ensure complete evaporation of ethanol, then it was removed and Mo-SnS was added to the mixture2Adding 0.1g of dimethyl silicone oil into PDMS, stirring uniformly, uniformly spin-coating the mixture on the conductive surface of ITO conductive glass by a spin-coating method, covering a layer of ITO conductive glass on the upper layer of the mixture to collect charges, applying pressure to the device by a stepper, and collecting piezoelectric signals by an oscilloscope.
Example 10
50mg of h-BN, 20mg of Mo (CO)6Placing in a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, and sealing the reaction kettleHeating to 150 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 4h, naturally cooling the product in the reaction kettle, collecting the product by a suction filtration method, and drying in a vacuum oven at 60 ℃ for 10h to obtain the final product Mo monatomic loaded h-BN (Mo-BN). Weighing a certain amount of final product Mo-BN, ultrasonically dispersing in ethanol, adding 1g of PDMS into the ethanol and Mo-BN mixed solution, stirring for 0.5h on a magnetic stirrer to ensure that the Mo-BN is uniformly dispersed in the PDMS, then putting the mixture into a vacuum oven, drying for 6h at 80 ℃ to ensure that the ethanol is completely evaporated, then taking out the ethanol, then adding 0.1g of dimethyl silicone oil into the PDMS mixed with the Mo-BN, uniformly stirring, then uniformly spin-coating the mixture on a conductive surface of ITO conductive glass by a spin-coating method, then covering a layer of ITO conductive glass on the conductive surface to collect charges, finally applying pressure to a device by a stepper, and collecting piezoelectric signals by an oscilloscope.
Example 11
50mg of h-BN, 20mg of Cr (CO) are weighed out6Placing the mixture into a 25ml high-temperature reaction kettle, adding 15ml of toluene and oleylamine mixed solution into the reaction kettle, sealing the reaction kettle, heating to 150 ℃ at a heating rate of 10 ℃/min, keeping the temperature for 4 hours, naturally cooling a product in the reaction kettle, collecting the product by a suction filtration method, and drying in a vacuum oven at 60 ℃ for 10 hours to obtain the final product Cr monatomic-loaded h-BN (Cr-BN). Weighing a certain amount of final product Mo-BN, ultrasonically dispersing in ethanol, adding 1g of PDMS into the mixed solution of ethanol and Cr-BN, stirring for 0.5h on a magnetic stirrer to ensure that the Cr-BN is uniformly dispersed in the PDMS, then putting the mixture into a vacuum oven, drying for 6h at 80 ℃ to ensure that the ethanol is completely evaporated, then taking out the ethanol, then adding 0.1g of dimethyl silicone oil into the PDMS mixed with the Cr-BN, uniformly stirring, then uniformly spin-coating the mixture on a conductive surface of ITO conductive glass by a spin-coating method, then covering a layer of ITO conductive glass on the conductive surface to collect charges, finally applying pressure to a device by a stepper, and performing wave indicationThe device collects the piezoelectric signal.
Comparative example 1
Weighing a certain amount of original BN (h-BN), ultrasonically dispersing in ethanol, adding 1g of PDMS into the mixed solution of the ethanol and the original BN, stirring for 0.5h on a magnetic stirrer to ensure that the original BN is uniformly dispersed in the PDMS, then putting the mixture into a vacuum oven, drying for 6h at 80 ℃ to ensure that the ethanol is completely evaporated, then taking out the mixture, then adding 0.1g of dimethicone into the PDMS mixed with the W-BN, uniformly stirring, then uniformly spin-coating the mixture on a conductive surface of ITO conductive glass by a spin-coating method, then covering a layer of ITO conductive glass on the conductive surface to collect charges, finally applying pressure to a device by a stepper, and collecting piezoelectric signals by an oscilloscope. The piezoelectric performance of the piezoelectric device prepared in this comparative example under a pressure of 18N is shown in fig. 2.
Comparative example 2
Weighing 1g of PDMS, adding 0.1g of dimethyl silicone oil, stirring uniformly, uniformly spin-coating the mixture on the conductive surface of ITO conductive glass by a spin-coating method, covering a layer of ITO conductive glass on the mixture to collect charges, applying pressure to the device by a stepper, and collecting piezoelectric signals by an oscilloscope. The piezoelectric performance of the piezoelectric device prepared in this comparative example under a pressure of 18N is shown in fig. 2.
The invention discloses a method for improving the piezoelectric performance of a material, and demonstrates an efficient monatomic piezoelectric material. The metal monatomic is coordinated with atoms on the surface of the piezoelectric material and combined, so that the potential on the surface of the piezoelectric material is generated, and the polarizability is increased under the condition of mechanical external force, and the performance of the piezoelectric material is improved by about 10 times by taking the monatomic loaded h-BN nanosheet as an example. The method can provide a novel research method for the piezoelectric material to improve the piezoelectric performance and the mechanism research.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
It should be understood that the technical solution of the present invention is not limited to the above-mentioned specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention without departing from the spirit of the present invention and the protection scope of the claims.
Claims (10)
1. A method for preparing a monatomic piezoelectric material, characterized by comprising:
at least carrying out hydrothermal reaction on the piezoelectric material and a metal monatomic source at 140-180 ℃ to obtain the monatomic piezoelectric material.
2. The method of claim 1, wherein: the piezoelectric material comprises h-BN and MoS2、SnS2、MoSe2、SnO2、WS2、CrTe2Any one or a combination of two or more of them; preferably, the piezoelectric material is a two-dimensional piezoelectric material;
and/or the metal monatomic source comprises a metal inorganic substance and/or a metal organic substance; preferably, the metal forming the metal inorganic substance and/or the metal organic substance includes any one or a combination of two or more of W, Cr, Co, Pt, Mo, Ni, Pd, and Rh; preferably, the metalorganic comprises a metal carbonyl organic complex; preferably, the source of metal monatomic comprises W (CO)6、W(CO)4、Cr(CO)6、Ni(CO)4、Mo(CO)6、Na2WO4Any one or a combination of two or more of them; particularly preferred is W (CO)6。
3. The production method according to claim 1, characterized by comprising: mixing the piezoelectric material with a metal monatomic source and a solvent, and then carrying out the hydrothermal reaction for 2-6 h;
preferably, a piezoelectric material, a metal monatomic source and a solvent are mixed to form a hydrothermal reaction system, and then the temperature of the hydrothermal reaction system is increased to 140-180 ℃ at a heating rate of 5-10 ℃/min and a hydrothermal reaction is carried out to prepare the monatomic piezoelectric material;
preferably, the solvent comprises a mixed solvent of toluene and oleylamine;
and/or, the preparation method further comprises the following steps: after the hydrothermal reaction is finished, washing, separating and drying the obtained mixture;
preferably, the washing solvent used in the washing treatment comprises any one or a combination of two or more of ethanol, n-hexane, cyclohexane, ethanol and chloroform; preferably, the drying treatment is carried out at the temperature of 40-80 ℃ for 6-10 h.
4. A monatomic piezoelectric material produced by the method described in any one of claims 1 to 3;
preferably, the monatomic piezoelectric material comprises a piezoelectric material serving as a carrier and a metal monatomic loaded on the surface of the carrier, wherein the metal monatomic is loaded on the surface of the carrier through chemical bonding with atoms on the surface of the carrier;
preferably, the content of the metal monoatomic atom in the monoatomic piezoelectric material is 1.5-2.5 wt%.
5. Use of the monatomic piezoelectric material according to claim 4 for the production of a piezoelectric device.
6. A method of manufacturing a piezoelectric device, comprising:
preparing a monatomic piezoelectric material by the method according to any one of claims 1 to 3;
and uniformly mixing the monatomic piezoelectric material, the packaging material and the curing agent, then applying the obtained mixture to the surface of a conductive substrate, and forming the piezoelectric device through assembly.
7. The method according to claim 6, comprising:
mixing the monatomic piezoelectric material with a dispersing agent to form monatomic piezoelectric material dispersion liquid, adding a packaging material, uniformly mixing, and then drying to obtain a mixture of the monatomic piezoelectric material and the packaging material;
uniformly mixing the mixture of the monatomic piezoelectric material and the packaging material with a curing agent, then applying the obtained mixture to a conductive surface of a conductive substrate, and forming the piezoelectric device through assembly;
preferably, the encapsulating material comprises polydimethylsiloxane;
preferably, the dispersant comprises ethanol and/or acetone;
preferably, the curing agent comprises hydrogen-containing silicone oil; preferably, the curing agent comprises dimethicone;
preferably, the conductive substrate comprises conductive glass, preferably single-sided conductive glass; more preferably, the single-sided conductive glass comprises any one or a combination of more than two of ITO conductive glass, FTO conductive glass and PET-ITO conductive film, wherein the single side of the ITO conductive glass is plated with indium tin oxide;
preferably, the preparation method comprises the following steps: applying the obtained mixture to a conductive surface of conductive glass by adopting a spin coating and/or spray coating mode and forming a piezoelectric device by assembling; preferably, the preparation method comprises the following steps: spin-coating the obtained mixture on the conductive surface of the conductive glass at a spin-coating speed of 600-1200 rpm, and assembling to form a piezoelectric device;
preferably, the mass ratio of the packaging material to the curing agent is 10-20: 1.
8. A piezoelectric device prepared by the method of claim 6 or 7, comprising a first conductive glass layer, a piezoelectric material layer, and a second conductive glass layer arranged in this order along a set direction, the piezoelectric material layer being formed by curing the monatomic piezoelectric material with an encapsulating material.
9. A piezoelectric device according to claim 8, wherein: the first conductive glass layer and the second conductive glass layer are both single-sided conductive glass; preferably, the single-sided conductive glass comprises any one or a combination of more than two of ITO conductive glass, FTO conductive glass and a PET-ITO conductive film, wherein the single side of the ITO conductive glass is plated with indium tin oxide;
and/or the conductive surfaces of the first conductive glass layer and the second conductive glass layer are arranged in contact with the piezoelectric material layer;
and/or the thickness of the piezoelectric material layer is 0.4-0.6 mm.
10. A method of enhancing the performance of a piezoelectric material, comprising: at least enabling a piezoelectric material and a metal monatomic source to carry out hydrothermal reaction at 140-180 ℃, so that the piezoelectric material is loaded with metal monatomics;
preferably, the piezoelectric material is mixed with a metal monatomic source and a solvent, and then the hydrothermal reaction is performed;
more preferably, the piezoelectric material, the metal monatomic source and the solvent are mixed to form a hydrothermal reaction system, and then the temperature of the hydrothermal reaction system is increased to 140-180 ℃ at a heating rate of 5-10 ℃/min to carry out the hydrothermal reaction;
preferably, the piezoelectric material comprises h-BN and MoS2、SnS2、MoSe2、SnO2、WS2、CrTe2Any one or a combination of two or more of them; more preferably, the piezoelectric material is a two-dimensional piezoelectric material;
preferably, the metal monatomic source comprises a metal inorganics and/or a metal organics; more preferably, the metal forming the metal inorganic substance and/or the metal organic substance includes any one or a combination of two or more of W, Cr, Co, Pt, Mo, Ni, Pd, and Rh; more preferably, the metalorganic comprises a metal carbonyl organic complex; more preferably, the source of metal monatomic comprises W (CO)6、W(CO)4、Cr(CO)6、Ni(CO)4、Mo(CO)6、Na2WO4Any one or a combination of two or more of them; particularly preferred is W (CO)6；
Preferably, the solvent comprises a mixed solvent of toluene and oleylamine;
preferably, after the hydrothermal reaction is finished, washing, separating and drying the obtained mixture; more preferably, the washing solvent used in the washing treatment includes any one or a combination of two or more of ethanol, n-hexane, cyclohexane, ethanol and chloroform; more preferably, the drying treatment is carried out at the temperature of 40-80 ℃ for 6-10 h.
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