CN114639771A - Preparation method of high-performance self-powered acoustic sensor based on piezoelectric nanorods - Google Patents
Preparation method of high-performance self-powered acoustic sensor based on piezoelectric nanorods Download PDFInfo
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01H—MEASUREMENT OF MECHANICAL VIBRATIONS OR ULTRASONIC, SONIC OR INFRASONIC WAVES
- G01H11/00—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties
- G01H11/06—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties by electric means
- G01H11/08—Measuring mechanical vibrations or ultrasonic, sonic or infrasonic waves by detecting changes in electric or magnetic properties by electric means using piezoelectric devices
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/04—Treatments to modify a piezoelectric or electrostrictive property, e.g. polarisation characteristics, vibration characteristics or mode tuning
- H10N30/045—Treatments to modify a piezoelectric or electrostrictive property, e.g. polarisation characteristics, vibration characteristics or mode tuning by polarising
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
- H10N30/07—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base
- H10N30/074—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by depositing piezoelectric or electrostrictive layers, e.g. aerosol or screen printing
- H10N30/077—Forming of piezoelectric or electrostrictive parts or bodies on an electrical element or another base by depositing piezoelectric or electrostrictive layers, e.g. aerosol or screen printing by liquid phase deposition
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Abstract
The invention discloses a preparation method of a high-performance self-powered acoustic sensor based on piezoelectric nanorods. The method can obtain a piezoelectric layer and a patterned electrode layer with uniformly distributed bar-shaped materials in the inner part. The uniform distribution is realized by spin coating and blade coating, and the patterned electrode layer can be realized by printing, vacuum evaporation and screen printing. The method is simple and quick, saves cost, can prepare high-performance self-powered acoustic sensors in batches, and has higher sensitivity.
Description
Technical Field
The invention relates to the field of acoustic sensors, in particular to a preparation method of a high-performance self-powered acoustic sensor based on piezoelectric nanorods.
Background
Various sounds are ubiquitous in the natural world and in life and work of people, and the sound-electricity conversion device is widely applied to various fields such as environmental protection, industrial manufacturing, medical care, medical research, scientific research, military defense systems and the like. The piezoelectric acoustic sensor based on the piezoelectric material can directly convert a sound signal into an electric signal without an external power supply, is suitable for various application occasions, and is concerned by researchers due to the characteristics of good durability and the like.
In order to manufacture the piezoelectric acoustic sensor, researchers have tried a sol-gel method, an electrostatic spinning method, and a hot pressing method. The sol-gel method is generally suitable for ceramic materials with precursors, and has the defects of complex steps, time consumption, high cost, no universality and the like; the electrostatic spinning method is only suitable for the macromolecule-based material which can be dissolved in the solvent; the hot pressing method has the disadvantages of large investment and high cost.
Therefore, it has been one of the hot spots of research to develop a high-performance piezoelectric acoustic sensor suitable for various materials, and the preparation method is simple, fast and cost-effective.
Disclosure of Invention
The invention aims to overcome the defects of a high-performance self-powered acoustic sensor preparation technology and provides a preparation method of a high-performance self-powered acoustic sensor based on piezoelectric nanorods, and the method has the advantages of simplicity, rapidness, cost saving and large-scale preparation.
The invention relates to a preparation method of a high-performance self-powered acoustic sensor based on piezoelectric nanorods, which comprises the following steps:
1) preparing ink of the nano-rods: uniformly mixing the rod-shaped piezoelectric material and the polymer to obtain the piezoelectric nanorod polymer mixed ink for spin coating or blade coating;
2) preparing a piezoelectric layer: attaching the piezoelectric nanorod polymer mixed ink to a polymer substrate film with an electrode by a spin coating or blade coating method to prepare a piezoelectric layer with a certain thickness;
3) curing the piezoelectric layer: according to the characteristics of the high polymer material, selecting a curing condition and curing the piezoelectric layer;
4) polarizing the piezoelectric layer: placing the solidified piezoelectric layer in a high-voltage direct-current voltage and high-temperature environment for polarization;
5) preparing an electrode: according to the requirements of the sensor, a conductive material is used for preparing a patterned electrode on the surface of the polarized piezoelectric layer by evaporation or by using electrode ink by a printing or silk-screen printing method;
6) assembling a sensor: the patterned electrode is drawn out with a conductive filament, resulting in a usable acoustic sensor.
According to the present invention, the rod-shaped piezoelectric material in the step 1) may be lead zirconate titanate (s: (PZT), Barium Titanate (BT), bismuth sodium titanate (BNT), potassium sodium niobate (KNN), bismuth ferrite (BiFeO)3) Alumina (Al)2O3) One or more of aluminum nitride (AlN), indium nitride (InN) and gallium nitride (GaN) and derived solid solutions thereof.
According to the invention, the polymer in step 1) can be one of silicone rubber prepolymer, polyurethane prepolymer, self-crosslinking polyacrylate prepolymer, self-crosslinking epoxy resin prepolymer, acrylated epoxy resin, unsaturated polyester, polyurethane acrylate, organic silicon oligomer and photo-curing resin containing photo-polymerization initiator.
According to the invention, the mass fraction of the rod-shaped piezoelectric material in the polymer mixed ink in the step 1) is 0-90% and is not 0.
According to the invention, the thickness of the piezoelectric layer in the step 2) is 0-10 cm and is not 0.
According to the invention, the polymer substrate film in the step 2) is one of high polymer materials such as polyethylene terephthalate, polyimide, polystyrene, polyethylene, polypropylene, polyvinyl chloride and polybenzimidazole and derivatives thereof.
According to the invention, the curing temperature in the step 3) is 0-300 ℃, and for the photo-curing resin system, a light source used for photo-curing is at least one of visible light, laser, infrared light, ultraviolet light, X-ray, electron beams and ion beams.
According to the invention, in the step 4), the polarization temperature is 20-200 ℃, the polarization time is 0-72 h and is not 0, and the polarization voltage is 0-500 kV/mm and is not 0.
According to the invention, the conductive material in the step 5) is one or more of metal, metal oxide and carbon material.
The metal is gold, silver or copper.
The metal oxide is indium tin oxide.
The carbon material is carbon-based material such as graphite alkyne, graphene, carbon nano tube or graphite.
According to the present invention, the electrode ink in step 5) is a solution of a metal nanomaterial or a carbon material.
The metal nano material is a conductive material such as nano gold or nano silver.
According to the invention, the conductive filament in step 6) is a conductive material such as an aluminum filament, a gold filament or a silver filament.
Compared with the prior art, the invention has the following advantages:
1) the method is simple and quick by a spin coating or blade coating method, can prepare high-performance self-powered acoustic sensors in batches, and saves the cost;
2) the preparation method has wide universality, and the sensor also has higher sensitivity.
Drawings
FIG. 1 is a schematic view of a method for manufacturing a high-performance self-powered acoustic sensor based on piezoelectric nanorods according to the present invention;
figure 2 is a cross-sectional SEM image of a cured piezoelectric layer prepared in example 1 of the present invention;
figure 3 is an enlarged SEM image of a cross-section of a cured piezoelectric layer prepared in example 1 of the present invention;
FIG. 4 is a diagram of a piezoelectric acoustic sensor fabricated in example 1 of the present invention;
FIG. 5 is a graph of the output voltage of the piezoelectric acoustic sensor prepared in example 1 of the present invention (fixed frequency acoustic stimulation);
fig. 6 is a graph of the output voltage of the piezoelectric acoustic sensor prepared in example 1 of the present invention (music stimulation);
fig. 7 is a graph of the output voltage of the piezoelectric acoustic sensor prepared in embodiment 1 of the present invention (real human voice stimulation);
fig. 8 is a fourier transform graph (real voice stimulation) of the output voltage of the piezoelectric acoustic sensor prepared in example 1 of the present invention;
fig. 9 shows the results of the frequency selectivity test of the piezoelectric acoustic sensor manufactured in example 2 of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
(1) Preparation of a polarizing electrode: preparing gold-covered polyethylene terephthalate films as polarized upper and lower electrodes by using a vacuum evaporation method, wherein the deposition thickness of gold is 100 nm, and the area of each polarized electrode is 2cm multiplied by 3 cm;
(2) preparing ink of the nano-rods: mixing a potassium-sodium niobate nanorod with a polydimethylsiloxane prepolymer and a polydimethylsiloxane curing agent in a mass ratio of 10:1, and then putting the mixture into an ice-water bath to stir for 0.5h to mix uniformly, wherein the content of the potassium-sodium niobate nanorod in the ink is 60%; the specific dosage is 2.4g of potassium-sodium niobate nano-rod, 1.6g of polydimethylsiloxane prepolymer and 0.16g of polydimethylsiloxane curing agent;
(3) preparing a piezoelectric layer: fixing the lower electrode on a spin coater platform with the surface with the metal gold facing upwards, sucking ink by a suction pipe, dripping the ink on the lower electrode, and preparing a piezoelectric layer by spin coating at the spin coating speed of 3000 rpm for 30 s; spin-coating an adhesive solution consisting of a polydimethylsiloxane prepolymer and a polydimethylsiloxane curing agent in a mass ratio of 10:1 on one surface of an upper electrode with metal gold to obtain an adhesive upper electrode, wherein the spin-coating speed is 4500 rpm, and the spin-coating time is 30 s;
(4) curing the piezoelectric layer: covering one surface of the upper electrode adhesion layer on the piezoelectric layer of the lower electrode, and standing at 80 ℃ for 2h until the upper electrode adhesion layer is completely cured;
(5) polarizing the piezoelectric layer: placing the solidified piezoelectric layer at 1 kV voltage, and polarizing for 12h at 150 ℃; after polarization, tearing off the upper and lower electrodes to obtain a polarized piezoelectric layer;
(6) preparing an electrode: placing the polarized piezoelectric layer under a mask plate, using gold as an electrode material, and obtaining electrode patterns with the thickness of 100 nm on the upper surface and the lower surface of the piezoelectric layer in a vacuum coating mode;
(7) assembling a sensor: and (3) respectively connecting the conductive silver paint and two conductive silver wires with the length of 10cm and the diameter of 0.1mm with the upper and lower surface electrodes of the piezoelectric layer with the electrodes in the step (6) to obtain the high-performance acoustic sensor for performance test.
And performing acoustoelectric performance test on the prepared high-performance self-powered acoustic sensor, wherein the effective area which can contact sound in the test is 1.6 cm multiplied by 2.4 cm. During testing, an audio file with a fixed frequency of 250 Hz is firstly played under the condition of 108 dB, the distance between the sensor and a sound source is 2cm, the output voltage of the sensor is 330 mV, and the audio file is obtained according to a calculation formula of the sensitivity of the acoustic-electric sensor
WhereinSWhich is indicative of the sensitivity of the sensor,Vis the output voltage of the sensor and is,P 0 is a reference sound pressure of 0.00002 Pa,L p is a value measured by a decibel meter.
The sensitivity of the high-performance acoustic sensor is 47.25 mV/Pa. Then, playing a section of light music audio under the condition of 100dB, wherein the electric signal acquired by the sensor is almost the same as the original signal of the audio; finally, the person speaks English letters A to G respectively towards the sensor, Fourier transform is carried out on the voltage signals collected by the sensor, and the result shows that the electric signals output by the high-performance acoustic sensor are obviously different in time domain and frequency domain and can be used for distinguishing different letters.
Example 2
(1) Preparation of a polarizing electrode: preparing silver-covered polyethylene terephthalate films as polarized upper and lower electrodes by using a vacuum evaporation method, wherein the deposition thickness of silver is 100 nm, and the area of the polarized electrode is 4cm multiplied by 4 cm;
(2) preparing ink of the nano-rods: mixing barium titanate nanorods with Ecoflex00-30 prepolymer and Ecoflex00-30 curing agent in a mass ratio of 1:1, and then putting the mixture into an ice water bath to be stirred for 0.5h to be uniformly mixed, wherein the content of the barium titanate nanorods in the ink is 40%; the specific dosage is 2.0g of barium titanate nano rod, 1.5g of Ecoflex00-30 prepolymer and 1.5g of Ecoflex00-30 curing agent;
(3) preparing a piezoelectric layer: the surface of the lower electrode with the metal silver faces upwards, the lower electrode is fixed on a platform of a spin coater, ink is absorbed by a suction tube and is dripped on the lower electrode, and a piezoelectric layer is prepared by spin coating at the spin coating speed of 3500 rpm for 30 s; spin-coating adhesive liquid consisting of Ecoflex00-30 prepolymer and Ecoflex00-30 curing agent in a mass ratio of 1:1 on the surface of an upper electrode with metal silver to obtain an upper electrode with adhesion, wherein the spin-coating speed is 5000rpm, and the spin-coating time is 30 s;
(4) curing the piezoelectric layer: covering one surface of the upper electrode adhesion layer on the piezoelectric layer of the lower electrode, and standing at 100 ℃ for 2h until the upper electrode adhesion layer is completely cured;
(5) polarizing the piezoelectric layer: placing the solidified piezoelectric layer at 0.8 kV voltage, and polarizing for 72h at 30 ℃; after polarization, tearing off the upper and lower electrodes to obtain a polarized piezoelectric layer;
(6) preparing an electrode: taking the solidified piezoelectric layer as a printing substrate, wherein the size of the printing substrate is 4cm multiplied by 4 cm; injecting 3g of nano-silver ink into a printer ink box of an Ultimus I pneumatic fluid dispensing system controlled by 2400 multiaxial mobile platforms of Nordson EFD company, fixing the piezoelectric layer in the step (5) on a printing platform by using a printer ink box with a diameter of 200
The printing nozzle directly writes electrode ink on a printing substrate at the speed of 10mm/s under the air pressure of 10psi according to image-text information, and electrodes are formed on the upper surface and the lower surface of the piezoelectric layer;
(7) assembling a sensor: cutting the piezoelectric layer with the electrodes in the step (6) into 5 rectangles with different length-width ratios, and respectively recording the rectangles as channels 1-5; the specific implementation method comprises the following steps: 15mm × 5mm (lane 1), 13mm × 5mm (lane 2), 11mm × 5mm (lane 3), 9mm × 5mm (lane 4), 7mm × 5mm (lane 5); fixing the 5 different rectangular piezoelectric layers on the polymethyl methacrylate with a hollow structure, wherein two adjacent rectangular piezoelectric layers are not connected; and (3) respectively connecting the conductive silver paint and 10 conductive gold wires with the length of 10cm and the diameter of 0.1mm with the upper and lower surface electrodes of the piezoelectric layer to obtain the high-performance acoustic sensor for performance test.
The prepared high-performance acoustic sensor is subjected to acoustoelectric performance test, a 100 Hz-1000 Hz frequency sweeping signal is played under the condition that the sound pressure is 100dB, the laser Doppler vibrometer is adopted to test the resonance frequency of the sensor at different channel positions, the test result shows that piezoelectric films in different shapes have different resonance frequencies, the frequency selection can be realized, and the piezoelectric acoustic sensor prepared by the method can be used in the field of artificial cochlea.
Example 3
(1) Preparation of a polarizing electrode: preparing a polyimide film covered by gold as polarized upper and lower electrodes by using a vacuum evaporation method, wherein the deposition thickness of the gold is 100 nm, and the area of the polarized electrode is 2cm multiplied by 2.5 cm;
(2) preparing ink of the nano-rods: mixing lead zirconate titanate nanorods with polyurethane acrylate, and then putting the mixture into an ice water bath to stir for 0.5h to mix uniformly, wherein the content of the lead zirconate titanate nanorods in the ink is 30%; the specific dosage is 1.5g of lead zirconate titanate nano rod and 3.5 g of urethane acrylate;
(3) preparing a piezoelectric layer: fixing the lower electrode on a spin coater platform with the surface with the metal gold facing upwards, sucking ink by a suction pipe, dripping the ink on the lower electrode, and preparing a piezoelectric layer by spin coating at the spin coating speed of 500 rpm for 30 s; spin-coating urethane acrylate on the surface of the upper electrode with the metal gold to obtain an upper electrode with adhesiveness, wherein the spin-coating speed is 2000rpm, and the spin-coating time is 30 s;
(4) curing the piezoelectric layer: covering the surface of the upper electrode with the polyurethane acrylate on the piezoelectric layer of the lower electrode, and placing under a 405nm and 150W ultraviolet lamp for photocuring for 30 min;
(5) polarizing the piezoelectric layer: placing the solidified piezoelectric layer at 2kV voltage, and polarizing for 24h at 100 ℃; after polarization, tearing off the upper and lower electrodes to obtain a polarized piezoelectric layer;
(6) preparing an electrode: printing electrodes on the upper and lower surfaces of the piezoelectric layer obtained in (5) by a screen printing method using silver ink;
(7) assembling a sensor: and (4) respectively connecting a copper adhesive tape and two conductive aluminum wires with the length of 10cm and the diameter of 0.1mm with the upper surface electrode and the lower surface electrode of the piezoelectric layer with the electrodes in the step (6), and leading out the electrodes on the surface of the sensor to obtain the high-performance acoustic sensor for performance test.
Claims (10)
1. A preparation method of a high-performance self-powered acoustic sensor based on piezoelectric nanorods is characterized by comprising the following steps:
1) preparing ink of the nano-rods: uniformly mixing the rod-shaped piezoelectric material and the polymer to obtain the piezoelectric nanorod polymer mixed ink for spin coating or blade coating;
2) preparing a piezoelectric layer: attaching the piezoelectric nanorod polymer mixed ink to a polymer substrate film with an electrode by a spin coating or blade coating method to prepare a piezoelectric layer with a certain thickness;
3) curing the piezoelectric layer: according to the characteristics of the high polymer material, selecting a curing condition and curing the piezoelectric layer;
4) polarizing the piezoelectric layer: placing the solidified piezoelectric layer in a high-voltage direct-current voltage and high-temperature environment for polarization;
5) preparing an electrode: according to the requirements of the sensor, a conductive material is used for preparing a patterned electrode on the surface of the polarized piezoelectric layer by evaporation or by using electrode ink by a printing or silk-screen printing method;
6) assembling a sensor: the patterned electrode is drawn out with a conductive filament, resulting in a usable acoustic sensor.
2. The preparation method according to claim 1, wherein the rod-shaped piezoelectric material in step 1) is one or more of lead zirconate titanate, barium titanate, sodium bismuth titanate, sodium potassium niobate, bismuth ferrite, aluminum oxide, aluminum nitride, indium nitride, gallium nitride and derived solid solutions thereof; the polymer is one of silicone rubber prepolymer, polyurethane prepolymer, self-crosslinking polyacrylate prepolymer, self-crosslinking epoxy resin prepolymer, acrylated epoxy resin, unsaturated polyester, polyurethane acrylate, organic silicon oligomer and light-curing resin containing a light polymerization initiator; the mass fraction of the rod-shaped piezoelectric material in the polymer mixed ink is 0-90% and is not 0.
3. The method according to claim 1, wherein the thickness of the piezoelectric layer in the step 2) is 0 to 10cm and is not 0.
4. The method according to claim 1, wherein the polymer base film in step 2) is one of polyethylene terephthalate, polyimide, polystyrene, polyethylene, polypropylene, polyvinyl chloride, and polybenzimidazole and derivatives thereof.
5. The preparation method according to claim 1, wherein the curing temperature in step 3) is 0 to 300 ℃, and a light source for photocuring the photocurable resin system is at least one of visible light, laser, infrared light, ultraviolet light, X-ray, electron beam and ion beam.
6. The method according to claim 1, wherein the polarization temperature in step 4) is 20 to 200 ℃, the polarization time is 0 to 72 hours and is not 0, and the polarization voltage is 0 to 500 kV/mm and is not 0.
7. The preparation method according to claim 1, wherein the conductive material in step 5) is one or more of a metal, a metal oxide and a carbon material; the electrode ink is a solution of a metal nano material or a carbon material.
8. The production method according to claim 7, wherein the metal is gold, silver, or copper; the metal oxide is indium tin oxide; the carbon material is graphite alkyne, graphene, a carbon nano tube or a graphite carbon-based material; the metal nano material is a nano gold or nano silver conductive material.
9. The method according to claim 1, wherein the conductive filament in step 6) is an aluminum, gold or silver conductive material.
10. A high-performance self-powered acoustic sensor based on piezoelectric nanorods, prepared by the preparation method of any one of claims 1 to 9.
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| PCT/CN2022/126703 WO2023173743A1 (en) | 2022-03-17 | 2022-10-21 | One-dimensional metal-doped perovskite type niobate piezoelectric material and preparation method therefor and use thereof, and flexible sound-sensitive device and preparation method therefor |
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| WO2023173743A1 (en) * | 2022-03-17 | 2023-09-21 | 中国科学院化学研究所 | One-dimensional metal-doped perovskite type niobate piezoelectric material and preparation method therefor and use thereof, and flexible sound-sensitive device and preparation method therefor |
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| WO2023173743A1 (en) * | 2022-03-17 | 2023-09-21 | 中国科学院化学研究所 | One-dimensional metal-doped perovskite type niobate piezoelectric material and preparation method therefor and use thereof, and flexible sound-sensitive device and preparation method therefor |
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