CN110350081B - Multifunctional flexible piezoelectric composite film with ordered structure and preparation method thereof - Google Patents

Multifunctional flexible piezoelectric composite film with ordered structure and preparation method thereof Download PDF

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CN110350081B
CN110350081B CN201910535151.XA CN201910535151A CN110350081B CN 110350081 B CN110350081 B CN 110350081B CN 201910535151 A CN201910535151 A CN 201910535151A CN 110350081 B CN110350081 B CN 110350081B
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王一平
李雄杰
杨颖�
何亭睿
孙胜
盛云
陈朋
胡悫睿
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Nanjing University of Aeronautics and Astronautics
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    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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Abstract

The invention discloses a multifunctional flexible piezoelectric composite film with an ordered structure and a preparation method thereof, relates to the field of flexible piezoelectric materials, can prepare a flexible functional piezoelectric film with high sensitivity, and has the advantages of simple process and low cost. The invention comprises the following steps: dissolving polymer powder in a solvent, and dispersing piezoelectric single crystal micro-slabs in the solvent to respectively obtain a polymer solution and a piezoelectric single crystal micro-slab dispersion liquid; inserting the glass sheet into the polymer solution for standing, and drying the glass sheet; uniformly and slowly dripping the suspension of the piezoelectric monocrystal microchip onto the surface of an inclined glass sheet with a thin-layer polymer, allowing the suspension to flow on the surface of the polymer, and drying the glass sheet; and (4) executing in a circulating way until the surface of the glass sheet forms a multi-functional flexible piezoelectric composite film with a multi-layer ordered structure. The invention can be widely applied to the fields of intelligent wearable equipment, flexible robots, energy collection, biomedicine and the like.

Description

Multifunctional flexible piezoelectric composite film with ordered structure and preparation method thereof
Technical Field
The invention relates to the field of flexible piezoelectric materials, in particular to a multifunctional flexible piezoelectric composite film with an ordered structure and a preparation method thereof.
Background
In recent years, the fields of flexible wearable equipment and artificial intelligence are rapidly developed, and the requirement on a sensor as a core component is higher and higher, and the flexible sensor is mainly composed of functional films with special microstructures. The development of high-performance functional films is a prerequisite in the field of flexible sensors, and the performance of a functional film body is directly related to the intellectualization and the multifunctionalization of carriers such as robots, medical equipment, human prostheses, wearable equipment and the like, and is highly valued by multidisciplinary researchers. As early as 1991, t.r. jensen et al developed functionalized films with tactile function for covering the surface of a robot, which were capable of sensing and responding to external forces using an internal sensor array, but these functionalized films had poor versatility and stability, and after multiple uses, the sensitivity of the functionalized films to external force responses was significantly impaired. With the development of sensing technology, in 2004, tokyo university of japan developed a flexible functionalized thin film with tactile function, which was drawn to a molecular semiconductor crystal size and fabricated onto a substrate material, sensor formation array fabricated as a flexible and shape-changeable functionalized thin film that was used for a robot and was capable of measuring pressure and temperature simultaneously. However, since the sensor uses a resistive pressure sensor and the functionalized membrane is thin, the unit moment generated by the same applied force is small, and therefore, the functionalized membrane has poor sensitivity. Chinese invention CN107123470A developed a flexible and elastic functionalized film, which comprises a pre-stretched elastic substrate, an elastic linker and nanowires. The elastic connecting body is positioned between the pre-stretched elastic substrate and the nano wire, and the material part of the elastic connecting body is embedded into the nano wire to form a mixed transition region so as to enhance the bonding performance between layers. Although the functionalized film prepared by the invention has higher sensitivity, the preparation method of the functionalized film is more complex. In addition, CN108896219A of the present invention provides a flexible biomimetic functionalized thin film, wherein the sensing layer includes a piezoresistive layer and a thin film electrode, the piezoresistive layer has a porous structure, and the contact interface region between the piezoresistive layer and the thin film electrode is filled with an elastomer, the flexible biomimetic functionalized thin film can sense the existence of air flow and pressure, and the flexible biomimetic functionalized thin film has a certain mechanical stability.
From the composition and structure of the functional film, the sensor mainly has a capacitance type, a piezoresistive type and a friction sensing type, and besides the above, the research on the piezoelectric type functional film is very little. Piezoelectric pressure sensors are generally made by compounding a piezoelectric polymer or inorganic functional material with a polymer matrix. To date, many functional materials of micro-nano structure, such as BaTiO3Nanowire, Ge/Si nanowire, single-walled carbon nanotube (SWNT), and PZT nanorod array, the device has been demonstrated to be in a slight external pressure state (<10kPa) has a very high sensitivity. Although these efforts have been very effective in improving the sensitivity of functionalized thin films, the preparation of nanowires, nanorods and microarrays is complicated, less reproducible and costly. Therefore, a problem to be solved is becoming urgent.
Disclosure of Invention
The invention provides a multifunctional flexible piezoelectric composite film with an ordered structure and a preparation method thereof, which can be used for preparing a flexible functionalized piezoelectric film with high sensitivity, and the preparation method has the advantages of simple process and low cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a multifunctional flexible piezoelectric composite film with an ordered structure comprises the following steps:
s1, dissolving the polymer powder in a solvent, and dispersing the piezoelectric single crystal micro-slabs in the solvent to respectively obtain a polymer solution and a piezoelectric single crystal micro-slab dispersion liquid;
s2, inserting the glass sheet into the polymer solution for standing, and then drying the glass sheet to form a polymer coating on the surface of the glass sheet;
s3, uniformly and slowly dripping the suspension of the piezoelectric single crystal microchip onto the surface of the glass sheet to enable the piezoelectric single crystal microchip to be flatly laid and oriented on the surface of the polymer coating film in the direction of the crystal plane 00l, and then drying the glass sheet;
and S4, circularly executing S2-S3 until the surface of the glass sheet forms the multifunctional flexible piezoelectric composite film with an ordered structure.
Further, the preparation method of the multifunctional flexible piezoelectric composite film with the ordered structure further comprises the following steps:
plating a gold electrode on the multifunctional flexible piezoelectric composite film with the ordered structure through ion sputtering, and leading out wires from the upper surface and the lower surface;
and mixing polydimethylsiloxane and a curing agent in a weight ratio of 10:1, coating the mixture on the upper surface and the lower surface of an electrode in a spin coating manner, and drying and curing the mixture at 80 ℃ to obtain the assembled piezoelectric film.
Further, the polymer comprises polyvinyl alcohol, polyvinylidene fluoride-based copolymer, polylactic acid, polydimethylsiloxane, polyurethane, polyacrylic resin and polyolefin.
Further, the solvent includes one or more of water, N-dimethylene formamide, N-methyl pyrrolidone.
Further, the concentration of the polymer solution is 0.5-3 wt%.
Further, the piezoelectric material single crystal microchip includes a barium titanate single crystal microchip, a lead magnesium niobate-lead titanate single crystal microchip, a sodium niobate single crystal microchip, a potassium sodium niobate single crystal microchip, a lithium tantalate single crystal microchip, and a quartz single crystal microchip.
Furthermore, the thickness of the piezoelectric material single crystal microchip is 1nm to 100nm, and the length and the width are 1 mu m to 10 mu m.
Furthermore, the concentration of the piezoelectric monocrystal microchip dispersion liquid is 1-5 wt%.
Furthermore, the thickness of the assembled piezoelectric film is 1-1000 μm.
The invention also provides a multifunctional flexible piezoelectric composite film with an ordered structure, which is prepared by the preparation method.
The invention has the beneficial effects that:
the ordered organic/inorganic hybrid flexible piezoelectric composite film formed by the layer-by-layer self-assembly method has the characteristics of high sensitivity, short response time, stable structure and the like, and compared with the traditional capacitive, resistive and organic transistor type sensors, the functional film has the advantages of simple preparation method and avoidance of the use of expensive, difficult-to-process and complex-structure nano materials such as microarrays, nanowires or nanorods and the like.
In addition, the nano materials with the micro-nano structure have the problems of inevitable uneven distribution, low repeatability and the like in the processing process. The flat piezoelectric material single crystal micro-sheets are easy to be oriented and arranged on the surface of the polymer, the layers are similar to an organic/inorganic hybrid structure of mussel shells, the structure can improve the stability of the film, and the piezoelectric material single crystal micro-sheets oriented on the adjacent layers can play a complementary role, so that the functional film has high sensitivity and excellent mechanical property.
On the other hand, the functional film can convert the vibration of vocal cord muscles of a human body into an electric signal, generates a corresponding electric signal according to the difference of vocal cord sounds of the human body, has repeatability and high reliability, and has potential application in the field of voice recognition systems in artificial intelligence.
In addition, the functional film can also sense weak physiological signals of human bodies, such as pulse, heartbeat and motion conditions, and can play an important role in the field of biomedicine.
In conclusion, the functional film prepared by the invention has the advantages of high sensitivity, simple preparation method, low cost and the like, and provides possibility for practical application in the fields of wearable equipment and biomedicine.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a plan view of a microstructure of a multifunctional flexible piezoelectric composite film of an ordered structure;
FIG. 2 is a three-dimensional view of a microstructure of a multifunctional flexible piezoelectric composite film with an ordered structure;
fig. 3 is a plan view of the structure after encapsulation of the multifunctional flexible piezoelectric composite film of ordered structure.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be further described in detail with reference to the following detailed description.
Example 1:
first, 0.5g of polyvinylidene fluoride copolymer P (VDF-TrFE) powder was dissolved in 100mL of N, N-Dimethylformamide (DMF) solvent for use, and then 0.5g of BaTiO3Dispersing the monocrystal microchip into 50mL of DMF (N, N-dimethyl formamide N, N-Dimethylformamide) solvent, performing ultrasonic treatment and stirring to form a suspension of piezoelectric monocrystal microchip, inserting a clean glass sheet into the above solution P (VDF-TrFE), standing for 3 minutes, drying, and sucking 10mL of BaTiO with a dropper3And uniformly and slowly dripping the single crystal microchip suspension on the inclined glass sheet, and drying the glass sheet. The flow of dropping the single crystal microchip suspension and drying after inserting the glass sheet into the P (VDF-TrFE) solution is repeated for 150 times in this way, and the multifunctional flexible piezoelectric composite film with the ordered structure is formed, as shown in figures 1 and 2.
And (3) uniformly plating gold electrodes on the upper and lower surfaces of the composite film through magnetron sputtering, and leading out leads from the upper and lower surfaces. Then, polydimethylsiloxane and a curing agent are mixed according to the weight ratio of 10:1, the mixture is coated on the upper surface and the lower surface of an electrode in a spin coating mode, the mixture is cured for 10 hours in an oven at the temperature of 80 ℃, and the structure diagram after packaging is shown in fig. 3. And after the packaging is finished, testing the sensitivity of the device.
Example 2:
first 0.5g of PVA (polyvinyl alcohol) powder was dissolved in 100mL of deionized water for use, and then 0.5g of BaTiO was added3Dispersing the single crystal micro-sheets into 50mL deionized water, performing ultrasonic treatment and stirring to form a suspension of piezoelectric single crystal micro-sheets, then inserting clean glass sheets into the PVA aqueous solution, standing for 3 minutes, drying, and then sucking 10mL BaTiO by a dropper3And uniformly and slowly dripping the single crystal microchip suspension on the inclined glass sheet, and drying. The glass sheet is inserted into PVA solution and then dripped with the single crystal microchip turbid liquid to be driedRepeating for 150 times to form the multifunctional flexible piezoelectric composite film with the ordered structure.
And (3) uniformly plating gold electrodes on the upper and lower surfaces of the composite film through magnetron sputtering, and leading out leads from the upper and lower surfaces. Then, the polydimethylsiloxane and the curing agent are mixed according to the weight ratio of 10:1, the mixture is coated on the upper surface and the lower surface of the electrode in a spin coating mode, and the mixture is cured for 10 hours in an oven at the temperature of 80 ℃. And after the packaging is finished, testing the sensitivity of the device.
Example 3:
0.5g P (VDF-TrFE) powder was first dissolved in 100mL DMF solvent for use, and then 0.5g PbTiO was added3Dispersing the single crystal microchip into 50mL of DMF solvent, and performing ultrasonic treatment and stirring to form PbTiO3A suspension of single crystal microchip was prepared by inserting a clean glass plate into the above P (VDF-TrFE) solution, allowing it to stand for 3 minutes, drying it, and then sucking 10mL of PbTiO with a dropper3And uniformly and slowly dripping the single crystal microchip suspension on the inclined glass sheet, and drying. The flow of dropping the single crystal microchip suspension and drying after inserting the glass sheet into the P (VDF-TrFE) solution is repeated for 150 times in this way, and the multifunctional flexible piezoelectric composite film with the ordered structure is formed.
And (3) uniformly plating gold electrodes on the upper and lower surfaces of the electric composite film through magnetron sputtering, and leading out leads from the upper and lower surfaces. Then, the polydimethylsiloxane and the curing agent are mixed according to the weight ratio of 10:1, the mixture is coated on the upper surface and the lower surface of the electrode in a spin coating mode, and the mixture is cured for 10 hours in an oven at the temperature of 80 ℃. And after the packaging is finished, testing the sensitivity of the device.
Example 4:
0.5g of PVA powder was first dissolved in 100mL of deionized water for use, and then 0.5g of Pb (Mg) was added1/3Nb2/3)O3-PbTiO3Dispersing the single crystal micro-sheet into 50mL deionized water, and forming Pb (Mg) by ultrasonic and stirring1/3Nb2/3)O3-PbTiO3A suspension of single crystal micro-pieces, then inserting clean glass pieces into the above aqueous PVA solution, standing for 3 minutes, oven drying, and then sucking 10mL Pb (Mg) with a dropper1/3Nb2/3)O3-PbTiO3The single crystal microchip suspension is uniformly and slowly dripped into the inclined suspensionAnd (5) drying the glass sheet. The flow of dropping the single crystal microchip turbid liquid and drying after inserting the glass sheet into the PVA solution is repeated for 150 times in this way, and the multifunctional flexible piezoelectric composite film with the ordered structure is formed.
And (3) uniformly plating gold electrodes on the upper and lower surfaces of the composite film through magnetron sputtering, and leading out leads from the upper and lower surfaces. Then, the polydimethylsiloxane and the curing agent are mixed according to the weight ratio of 10:1, the mixture is coated on the upper surface and the lower surface of the electrode in a spin coating mode, and the mixture is cured for 10 hours in an oven at the temperature of 80 ℃. And after the packaging is finished, testing the sensitivity of the device.
Example 5:
first, 3g of polydimethylsiloxane was mixed uniformly with 0.3g of a curing agent for use, and then 0.5g of Pb (Mg) was added1/ 3Nb2/3)O3-PbTiO3Dispersing the single crystal micro-tablets into 50mL of DMF solvent, and carrying out ultrasonic agitation to form Pb (Mg)1/3Nb2/3)O3-PbTiO3A suspension of single crystal microchip, then inserting a clean glass plate into the above polydimethylsiloxane mixed sol, standing for 3 minutes, curing at 100 deg.C for 3 hours, and then sucking 10mL Pb (Mg) with a dropper1/3Nb2/3)O3-PbTiO3And uniformly and slowly dripping the single crystal microchip suspension on the inclined glass sheet, and drying. And (3) inserting the glass sheet into the polydimethylsiloxane solution, then dropwise adding the single crystal microchip suspension and drying, and repeating the process for 150 times to form the multifunctional flexible piezoelectric composite film with the ordered structure.
And (3) uniformly plating gold electrodes on the upper and lower surfaces of the composite film through magnetron sputtering, and leading out leads from the upper and lower surfaces. Then, the polydimethylsiloxane and the curing agent are mixed according to the weight ratio of 10:1, the mixture is coated on the upper surface and the lower surface of the electrode in a spin coating mode, and the mixture is cured for 10 hours in an oven at the temperature of 80 ℃. And after the packaging is finished, testing the sensitivity of the device.
Comparative example 1:
0.5g P (VDF-TrFE) powder was first dissolved in 100mL DMF solvent for use, and then 0.5g BaTiO3Dispersing the micron particles into 50mL of DMF solvent, and performing ultrasonic treatment and stirring to form BaTiO3Suspension of microparticles, then inserting clean glass sheetThe above P (VDF-TrFE) solution was allowed to stand for 3 minutes, dried, and then 10mL of BaTiO was pipetted3And uniformly and slowly dripping the micron particle suspension on the inclined glass sheet, and drying. And (3) inserting the glass sheet into a P (VDF-TrFE) solution, then dropwise adding a micron particle suspension, and drying, and repeating the process for 150 times to form the multifunctional flexible piezoelectric composite film with the ordered structure.
And (3) uniformly plating gold electrodes on the upper and lower surfaces of the composite film through magnetron sputtering, and leading out leads from the upper and lower surfaces. Then, the polydimethylsiloxane and the curing agent are mixed according to the weight ratio of 10:1, the mixture is coated on the upper surface and the lower surface of the electrode in a spin coating mode, and the mixture is cured for 10 hours in an oven at the temperature of 80 ℃. And after the packaging is finished, testing the sensitivity of the device.
Comparative example 2:
firstly, 0.5g P (VDF-TrFE) powder is dissolved in 100mL DMF solvent, then a clean glass sheet is inserted into the P (VDF-TrFE) solution, the solution is dried after standing for 3 minutes, the flow of inserting the glass sheet into the P (VDF-TrFE) solution and then drying is repeated for 150 times, and the flexible piezoelectric film is formed.
And uniformly plating gold electrodes on the upper and lower surfaces of the piezoelectric film through magnetron sputtering, and leading out leads on the upper and lower surfaces. Then, the polydimethylsiloxane and the curing agent are mixed according to the weight ratio of 10:1, the mixture is coated on the upper surface and the lower surface of the electrode in a spin coating mode, and the mixture is cured for 10 hours in an oven at the temperature of 80 ℃. And after the packaging is finished, testing the sensitivity of the device.
The sensitivity test results of the films prepared in the above examples and comparative examples are as follows:
TABLE 1 sensitivity and electrical response of different examples and comparative samples
Figure BDA0002100335230000091
The invention has the beneficial effects that:
the ordered organic/inorganic hybrid flexible piezoelectric composite film formed by the layer-by-layer self-assembly method has the characteristics of high sensitivity, short response time, stable structure and the like, and compared with the traditional capacitive, resistive and organic transistor type sensors, the functional film has the advantages of simple preparation method and avoidance of the use of expensive, difficult-to-process and complex-structure nano materials such as microarrays, nanowires or nanorods and the like.
In addition, the nano materials with the micro-nano structure have the problems of inevitable uneven distribution, low repeatability and the like in the processing process. The flat piezoelectric material single crystal micro-sheets are easy to orient and arrange on the surface of the polymer, the layers are similar to an organic/inorganic hybrid structure among mussel shells, the structure can improve the stability of the film, and the piezoelectric material single crystal micro-sheets oriented on the adjacent layers can play a complementary role, so that the functional film has high sensitivity.
On the other hand, the functional film can convert the vibration of vocal cord muscles of a human body into an electric signal, generates a corresponding electric signal according to the difference of vocal cord sounds of the human body, has repeatability and high reliability, and has potential application in the field of voice recognition systems in artificial intelligence.
In addition, the functional film can also sense weak physiological signals of human bodies, such as pulse, heartbeat and motion conditions, and can play an important role in the field of biomedicine.
In conclusion, the functional film prepared by the invention has the advantages of high sensitivity, simple preparation method, low cost and the like, and provides possibility for practical application in the fields of wearable equipment and biomedicine.
The above description is only for the specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (8)

1. A preparation method of a multifunctional flexible piezoelectric composite film with an ordered structure is characterized by comprising the following steps:
s1, dissolving polymer powder in a solvent, wherein the polymer comprises: polyvinylidene fluoride and/or polyvinylidene fluoride-based copolymers;
dispersing piezoelectric single crystal micro-tablets into a solvent, wherein the piezoelectric single crystal micro-tablets are made of barium titanate single crystal micro-tablets;
respectively obtaining a polymer solution and a piezoelectric single crystal microchip dispersion liquid;
s2, inserting the glass sheet into the polymer solution for standing, and then drying the glass sheet to form a polymer coating on the surface of the glass sheet;
s3, uniformly and slowly dripping the piezoelectric single crystal microchip dispersion liquid on the surface of a glass sheet to enable the piezoelectric single crystal microchip to be tiled and oriented on the surface of the polymer coating film in the direction of the crystal plane 00l, and then drying the glass sheet;
s4, and circularly executing S2-S3 until the surface of the glass sheet forms the multifunctional flexible piezoelectric composite film with the ordered structure.
2. The method for preparing the multifunctional flexible piezoelectric composite film with the ordered structure according to claim 1, further comprising:
plating gold electrodes on the upper surface and the lower surface of the multifunctional flexible piezoelectric composite film with the ordered structure through ion sputtering, and leading out a lead on the surface of the obtained gold electrode;
and mixing polydimethylsiloxane and a curing agent in a weight ratio of 10:1, coating the mixture on the surface of the gold electrode in a spin coating manner, and drying and curing the mixture at 80 ℃ to obtain the assembled piezoelectric film.
3. The method for preparing the multifunctional flexible piezoelectric composite film with the ordered structure according to claim 1, wherein the solvent comprises one or more of water, N-dimethylformamide and N-methylpyrrolidone.
4. The method for preparing the multifunctional flexible piezoelectric composite film with the ordered structure according to claim 1, wherein the concentration of the polymer solution is 0.5-3 wt%.
5. The method for preparing the multifunctional flexible piezoelectric composite film with the ordered structure according to claim 1, wherein the thickness of the piezoelectric single crystal microchip material is 1 nm-100 nm, and the length and the width are 1 μm-10 μm.
6. The method for preparing the multifunctional flexible piezoelectric composite film with the ordered structure according to claim 1, wherein the concentration of the piezoelectric single crystal microchip dispersion liquid is 1-5 wt%.
7. The method for preparing the multifunctional flexible piezoelectric composite film with the ordered structure according to claim 2, wherein the thickness of the assembled piezoelectric film is 1-1000 μm.
8. A multifunctional flexible piezoelectric composite film of an ordered structure, which is prepared by the preparation method of any one of claims 1 to 7.
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