CN113193107B - Monoatomic piezoelectric material and its preparing method and use - Google Patents
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Abstract
The invention discloses a monoatomic piezoelectric material and a preparation method and application thereof. The preparation method comprises the following steps: at least leading the piezoelectric material and the metal monatomic source to carry out hydrothermal reaction at 140-180 ℃ to prepare 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 means that when some materials are subjected to an external force along a certain direction, the structure of the material is subjected to microscopic deformation, a polarization phenomenon is generated in the material, and positive and negative opposite charges appear on two opposite surfaces of the material. 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 LiNbO 3 In contrast, BN piezoelectric film phase velocities are superior to these materialsThe 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 LiNbO 3 In 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-layer or even single-layer BN nanosheets, and researches show that the method can improve the piezoelectric performance when the number of BN layers is reduced, but 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 of the invention, 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 leading the piezoelectric material and the metal monatomic source to carry out hydrothermal reaction at 140-180 ℃ to prepare the monatomic piezoelectric material.
Further, the piezoelectric material comprises h-BN and MoS 2 、SnS 2 、MoSe 2 、SnO 2 、WS 2 、CrTe 2 Any 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 、Na 2 WO 4 And any one or a combination of two or more thereof, without being 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, applying the obtained mixture to the surface of a conductive substrate, and forming a 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 the piezoelectric material and the metal monatomic source are subjected to hydrothermal reaction at 140-180 ℃, so that the piezoelectric material is loaded with 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 SnS 2 、MoS 2 、SnO 2 、WS 2 、MoSe 2 、CrTe 2 Equal two-dimensional piezoelectric material, selected metalThe 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 monatomic materials and the research 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 embodiments or the description of 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 it is also possible for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a structural view of a piezoelectric device produced in embodiment 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 microscope image of the final product W monatomic-supported h-BN (W-BN) in example 1 of the 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 provide the technical solutions of the present invention, which will be clearly and completely described below. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to 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 the piezoelectric material and the metal monatomic source are subjected to hydrothermal reaction at 140-180 ℃ to prepare the monatomic piezoelectric material.
In some more specific embodiments, the piezoelectric material comprises h-BN, moS 2 、SnS 2 、MoSe 2 、SnO 2 、WS 2 、CrTe 2 And any one or a combination of two or more thereof, without being 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 、Na 2 WO 4 Any one or a combination of two or more of them; particularly preferably W (CO) 6 。
In some more specific embodiments, the preparation method comprises: 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 6h.
In some more specific embodiments, the method of making 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 temperature of the drying treatment is 40-80 ℃, and the 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 the embodiments of the present invention also provides a monoatomic piezoelectric material manufactured 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 the embodiments 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 monoatomic piezoelectric material with a dispersing agent to form a monoatomic piezoelectric material dispersion solution, adding a packaging material, uniformly mixing, and drying to obtain a mixture of the monoatomic piezoelectric material and the packaging material;
and uniformly mixing the mixture of the monoatomic 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 through 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 mixture obtained 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: the obtained mixture is spin-coated on the conductive surface of the conductive glass at a spin-coating speed of 600-1200 rpm and assembled to form the piezoelectric device.
Further, the spin-coating rotation speed is any one of 600rpm, 700rpm, 800rpm, 900rpm, 1100rpm, 1200 rpm.
Furthermore, 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 fabricating a piezoelectric device specifically comprises:
and mixing the monatomic piezoelectric material and PDMS, adding a curing agent, stirring, and finally spin-coating, distributing on ITO conductive glass and assembling 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.
Further, the thickness of the piezoelectric material layer is 0.4-0.6 mm, and preferably 0.5mm.
In some more specific embodiments, the method for preparing the monatomic piezoelectric material specifically includes:
with h-BN nanosheet and W (CO) 6 As a raw material, a monatomic W-supported h-BN two-dimensional material (W-BN) was successfully prepared by a hydrothermal method of high-temperature high-pressure reaction 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 a piezoelectric material and a metal monatomic source are subjected to a hydrothermal reaction at 140 to 180 ℃, so that the piezoelectric material is loaded with metal monatomics.
In some more specific embodiments, the hydrothermal reaction is performed after mixing the piezoelectric material with a source of metal monatomic atoms 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, moS 2 、SnS 2 、MoSe 2 、SnO 2 、WS 2 、CrTe 2 Any 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 、Na 2 WO 4 Any one or a combination of two or more of them, 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 temperature of the drying treatment is 40-80 ℃, and the 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, 20mW of g (CO) 6 Placing 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 the monoatomic atom through a spherical aberration electron microscope image, and the successful loading of the monoatomic atom is indicated, as shown in figure 3, and the metal monoatomic atom is shown as a white dot in the image.
Weighing a certain amount of final product W-BN, ultrasonically dispersing in ethanol, adding 1g of PDMS into the mixed solution of ethanol and W-BN, 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 dimethyl silicone oil into the PDMS mixed with the W-BN, uniformly stirring, 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 of the ITO conductive glass 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) are weighed out 6 Placing 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 mixed solution of ethanol and W-BN, 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 the temperature of 80 ℃ to ensure that the ethanol is completely removedPervaporation is carried out, then the mixture is taken out, then 0.1g of dimethyl silicone oil is added into PDMS mixed with W-BN and is stirred uniformly, then the mixture is uniformly coated on the conductive surface of ITO conductive glass in a spinning mode, then a layer of ITO conductive glass is covered on the mixture to collect charges, finally, a stepping machine is used for applying pressure to the device, and piezoelectric signals are collected through an oscilloscope.
Example 3
50mg of h-BN, 60mg of W (CO) are weighed out 6 Placing 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 4
50mg of h-BN and 80mg of W (CO) are weighed out 6 Placing 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 is ultrasonically dispersed in ethanol, 1g of PDMS is added into the mixed solution of ethanol and W-BN and stirred on a magnetic stirrer for 0.5h to ensure that the W-BN is uniformly dispersed in the PDMS, then the mixture is placed into a vacuum oven and dried for 6h at the temperature of 80 ℃ to ensure that the ethanol is completely evaporated, then the mixture is taken out, then 0.1g of dimethicone is added into the PDMS mixed with the W-BN and stirred uniformly, then the mixture is uniformly coated on the conductive surface of ITO conductive glass by a coating method, then a layer of ITO conductive glass is covered on the conductive surface to collect electric charges, finally, the device is pressurized by a stepper, and piezoelectric signals are collected by an oscilloscope.
Example 5
50mg of h-BN, 100mg of W (CO) are weighed out 6 Placing 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 mixed solution of ethanol and W-BN, 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 dimethyl silicone oil into the PDMS mixed with the W-BN, uniformly stirring, 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 of the ITO conductive glass to collect electric charges to form a piezoelectric device (shown in figure 1), finally applying pressure on 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 weighed 2 50mg of Ni (CO) 4 Placing the mixture in a high temperature reaction of 25mlAdding 15ml of toluene and oleylamine mixed solution into a 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 MoS loaded with Ni monoatomic 2 (Ni-MoS 2 ). Weighing a certain amount of final product Ni-MoS 2 Ultrasonically dispersing in ethanol, and adding into the ethanol and Ni-MoS 2 1g PDMS was added to the mixed solution and stirred on a magnetic stirrer for 0.5h, ensuring Ni-MoS 2 Uniformly 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 mixture 2 Adding 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 mixture to collect charges, applying pressure to the device by a stepper, and collecting piezoelectric signals by an oscilloscope.
Example 7
50mg of MoS was weighed 2 100mg of Ni (CO) 4 Placing 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 MoS 2 (Ni-MoS 2 ). Weighing a certain amount of final product Ni-MoS 2 Ultrasonically dispersing in ethanol, and adding into the ethanol and Ni-MoS 2 1g PDMS was added to the mixed solution and stirred on a magnetic stirrer for 0.5h, ensuring Ni-MoS 2 Uniformly 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 mixture 2 In PDMS addAdding 0.1g of dimethyl silicone oil, stirring uniformly, uniformly spin-coating the mixture on a conductive surface of ITO conductive glass by a spin-coating method, covering a layer of ITO conductive glass on the conductive surface to collect charges, applying pressure to the device by a stepper, and collecting piezoelectric signals by an oscilloscope.
Example 8
50mg of SnS are weighed 2 50mg of Mo (CO) 4 Placing the mixture 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 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 SnS 2 (Mo-SnS 2 ). Weighing a certain amount of final product Mo-SnS 2 Ultrasonically dispersing in ethanol, and adding into the ethanol and Mo-SnS 2 1g PDMS was added to the mixed solution and stirred on a magnetic stirrer for 0.5h, ensuring that Mo-SnS 2 Uniformly 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 mixture 2 Adding 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 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 weighed 2 100mg of Mo (CO) 4 Placing 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 SnS 2 (Mo-SnS 2 ). Weighing a certain amount of final product Mo-SnS 2 Ultrasonically dispersing in ethanol, and adding into the ethanol and Mo-SnS 2 1g PDMS was added to the mixed solution and stirred on a magnetic stirrer for 0.5h, ensuring that Mo-SnS 2 Uniformly dispersed in PDMS, then the mixture was put into a vacuum oven and dried at 80 ℃ for 6h to ensure that the ethanol was completely evaporated, then it was taken out, and then Mo-SnS was added to the mixture 2 Adding 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) are weighed 6 And (2) placing 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 placing the product into a vacuum oven to dry for 10 hours at 60 ℃ to obtain a final product, namely the Mo monoatomic load 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 and 20mg of Cr (CO) are weighed 6 Placing the mixture in a 25ml high-temperature reaction kettleAdding 15ml of toluene and oleylamine mixed solution into a 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 supported 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, ensuring 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, 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 of the ITO conductive glass to collect charges, finally applying pressure to a device by a stepper, and collecting piezoelectric signals by an oscilloscope.
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 solutions of the present invention are not limited to the above specific embodiments, and any technical modifications made according to the technical solutions of the present invention fall within the protection scope of the present invention without departing from the spirit of the present invention and the scope of the claims.
Claims (16)
1. A method for preparing a monatomic piezoelectric material, characterized by comprising:
carrying out hydrothermal reaction on the piezoelectric material, a metal monatomic source and a mixed solvent of toluene and oleylamine at 140-180 ℃ to prepare the monatomic piezoelectric material;
wherein the piezoelectric material is selected from h-BN and MoS 2 、SnS 2 、MoSe 2 、SnO 2 、WS 2 、CrTe 2 Any one or a combination of two or more of them; the metal monatomic source is selected from W (CO) 6 、W(CO) 4 、Cr(CO) 6 、Ni(CO) 4 、Mo(CO) 6 、Na 2 WO 4 Any one or a combination of two or more of them.
2. The production method according to claim 1, characterized in that: the metal monatomic source is W (CO) 6 。
3. The production method according to claim 1, characterized by comprising: mixing a piezoelectric material, a metal monatomic source and a mixed solvent of toluene and oleylamine to form a hydrothermal reaction system, then heating the hydrothermal reaction system to 140-180 ℃ at a heating rate of 5-10 ℃/min, and carrying out hydrothermal reaction for 2-6 h to obtain the monatomic piezoelectric material.
4. The method for preparing according to claim 1, characterized by further comprising: after the hydrothermal reaction is finished, washing, separating and drying the obtained mixture;
wherein the washing solvent used for washing treatment is selected from one or more of ethanol, n-hexane, cyclohexane, ethanol and chloroform; the temperature of the drying treatment is 40-80 ℃, and the time is 6-10 h.
5. A monatomic piezoelectric material produced by the method described in any one of claims 1 to 4; 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; the content of metal single atoms in the single-atom piezoelectric material is 1.5 to 2.5wt%.
6. Use of the monatomic piezoelectric material according to claim 5 for the production of a piezoelectric device.
7. A method of manufacturing a piezoelectric device, comprising:
preparing a monatomic piezoelectric material using the method of any one of claims 1 to 4;
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.
8. The preparation method according to claim 7, characterized by specifically 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;
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.
9. The method for producing according to claim 8, characterized in that: the encapsulating material is selected from polydimethylsiloxane; the dispersant comprises ethanol and/or acetone; the curing agent is dimethyl silicone oil; the conductive substrate is single-sided conductive glass; the single-side conductive glass is selected from any one or the combination of more than two of ITO conductive glass, FTO conductive glass and PET-ITO conductive film, the single side of which is plated with indium tin oxide.
10. The method according to claim 8, characterized by comprising: applying the obtained mixture to the conductive surface of the conductive glass by adopting a spin coating and/or spray coating mode and forming a piezoelectric device through assembly; and spin-coating the obtained mixture on the conductive surface of the conductive glass at a spin-coating speed of 600-1200rpm, and assembling to form the piezoelectric device.
11. The method of claim 8, wherein: the mass ratio of the packaging material to the curing agent is 10 to 20.
12. A piezoelectric device produced by the method according to any one of claims 7 to 11, comprising a first conductive glass layer, a piezoelectric material layer, and a second conductive glass layer, which are disposed in this order along a set direction, the piezoelectric material layer being formed by curing the monatomic piezoelectric material with an encapsulating material.
13. A piezoelectric device according to claim 12, wherein: the first conductive glass layer and the second conductive glass layer are both single-sided conductive glass; the single-sided conductive glass is selected from any one or the combination of more than two of ITO conductive glass, FTO conductive glass and PET-ITO conductive film with indium tin oxide plated on the single side;
the conductive surfaces of the first conductive glass layer and the second conductive glass layer are arranged in contact with the piezoelectric material layer;
the thickness of the piezoelectric material layer is 0.4-0.6 mm.
14. A method of enhancing the performance of a piezoelectric material, comprising: mixing a piezoelectric material, a metal monoatomic source and a mixed solvent of toluene and oleylamine to form a hydrothermal reaction system, and then heating the hydrothermal reaction system to 140-180 ℃ at a heating rate of 5-10 ℃/min to carry out hydrothermal reaction, so that the piezoelectric material is loaded with metal monoatomic;
the piezoelectric material is selected from h-BN and MoS 2 、SnS 2 、MoSe 2 、SnO 2 、WS 2 、CrTe 2 Any one or a combination of two or more of them; said metal monatomic source is selected from W (CO) 6 、W(CO) 4 、Cr(CO) 6 、Ni(CO) 4 、Mo(CO) 6 、Na 2 WO 4 Any one or a combination of two or more of them.
15. The method of claim 14, wherein: the metal monatomic source is W (CO) 6 。
16. The method of claim 14, further comprising: after the hydrothermal reaction is finished, washing, separating and drying the obtained mixture; wherein the washing solvent used in the washing treatment is any one or a combination of more than two of ethanol, normal hexane, cyclohexane, ethanol and chloroform; the temperature of the drying treatment is 40-80 ℃, and the time is 6-10 h.
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