CN115849902A - Piezoelectric ceramic formula adapted to road vibration energy harvesting technology, preparation method and application thereof - Google Patents
Piezoelectric ceramic formula adapted to road vibration energy harvesting technology, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a piezoelectric ceramic formula adapted to a road energy harvesting technology, a preparation method and application thereof, wherein the piezoelectric ceramic formula mainly comprises a main component and additional components, and the main component comprises the following components: pb x Sr y Ba 1‑x‑y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1‑z O 3 Wherein: 0.7. Ltoreq. X.ltoreq.0.75, 0.02. Ltoreq. Y.ltoreq.0.06, 0.95. Ltoreq. Z.ltoreq.0.98, an additional component 0.2wt.% of CaCO based on the mass of the main component 3 And 0.05wt% CdCO 3 According to Pb x Sr y Ba 1‑x‑y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1‑z O 3 The preparation method comprises the steps of proportioning, pre-burning, secondary ball milling, molding, plastic removal, sintering, slicing, silver burning, polarization and the like in a chemical formula to prepare the ceramic wafer, the ceramic wafer is made into a piezoelectric transducer to be applied to a road, the optimal power generation performance is obtained under the condition that the road use condition is met, the piezoelectric ceramic with good piezoelectric performance, high electromechanical coupling coefficient and large dielectric constant is obtained, and a good foundation is laid for the development of the road piezoelectric energy harvesting technology.
Description
Technical Field
The invention relates to a piezoelectric ceramic formula suitable for a road vibration energy harvesting technology, a preparation method and application thereof.
Background
The road vibration energy harvesting technology based on the piezoelectric effect has the characteristics of high power-electricity conversion efficiency, simple structure, no electromagnetic interference and the like, can supply power for traffic facility monitoring equipment and wireless sensors, and realizes the whole life cycle monitoring of traffic facilities in a complex service environment. Various researchers have made a great deal of research based on a road vibration energy harvesting technology, including the structure of a piezoelectric transducer, a piezoelectric energy collecting circuit and piezoelectric transducer packaging. In the current actual measurement road test, the energy collection power density of the RPEH based on the improved drum structure can reach hundreds of watts per square meter, and the huge potential of the piezoelectric energy harvesting technology in the aspect of supplying power to the traffic auxiliary equipment is shown. The piezoceramic material plays an important role in energy collection as a core component of the piezoelectric transducer, and the lead zirconate titanate piezoceramic material becomes the most extensive piezoelectric material in a road piezoelectric acquisition device due to excellent piezoelectric and dielectric properties.
The piezoelectric ceramics are applied in a large area under a complex road service environment and need to meet two conditions so as to achieve the optimal power generation performance under the road condition. (1) The daily service temperature of a road is-10-80 ℃, and the piezoelectric property of the piezoelectric ceramic loses efficacy immediately when the ambient environment exceeds the Curie temperature, and the Curie temperature is generally specified to be twice of the ambient temperature in order to ensure the performance stability of the piezoelectric ceramic. (2) The piezoelectric charge constant is inversely proportional to the curie temperature, and the larger the piezoelectric charge constant of the ceramic is, the better the power generation performance is. The curie temperature of the ceramic needs to be satisfied by doping with an element to achieve the maximum piezoelectric charge constant. The research on the doping of ceramic elements is well-established, but the formula research on the piezoelectric ceramic under the action of road coupling is not related.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a piezoelectric ceramic formula adaptive to a road vibration energy harvesting technology and a preparation method thereof, so that the optimal power generation performance is obtained under the condition of meeting the road use condition, the piezoelectric ceramic with good piezoelectric performance, high electromechanical coupling coefficient and large dielectric constant is obtained, a good foundation is laid for the development of the road piezoelectric energy harvesting technology, and the piezoelectric ceramic formula can be applied to the technical field of road vibration energy harvesting.
In order to achieve the purpose, the invention provides the following technical scheme: a piezoelectric ceramic formula adapted to a road vibration energy harvesting technology mainly comprises main components and additional components, wherein the main components are as follows: pb x Sr y Ba 1-x-y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1-z O 3 Wherein: 0.7. Ltoreq. X.ltoreq.0.75, 0.02. Ltoreq. Y.ltoreq.0.06, 0.95. Ltoreq. Z.ltoreq.0.98, additional ingredients 0.2wt% of the mass of the main ingredients CaCO 3 And 0.05wt% CdCO 3 。
A preparation method of piezoelectric ceramics adaptive to a road vibration energy harvesting technology comprises the following steps:
s1: ingredients
Respectively and independently placing lead tetraoxide, titanium dioxide, barium dioxide, strontium carbonate, barium carbonate, antimony trioxide, niobium pentoxide, calcium carbonate and barium carbonate in an electric heating blast drying oven, drying at the temperature of 120-150 ℃ for 7 hours, and then forming Pb according to a raw material composition formula x Sr y Ba 1-x-y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1-z O 3 Wherein: x is more than or equal to 0.7 and less than or equal to 0.75, y is more than or equal to 0.02 and less than or equal to 0.06, z is more than or equal to 0.95 and less than or equal to 0.98, and CaCO accounts for 0.2wt% of the mass ratio of the main components 3 And 0.05wt% CdCo 3 Weighing and uniformly mixing, placing the raw materials in a planetary ball mill for ball milling for 7 hours, and then drying the raw materials;
s2: pre-firing
Placing the mixed powder into an alumina crucible, sealing the alumina crucible with a cover, placing the alumina crucible into a high-temperature pre-sintering furnace for pre-sintering, and synthesizing for 2.5 hours after heating to 960-1000 ℃;
s3: secondary ball milling
Grinding the block powder after pre-sintering, adding 10% polyvinyl alcohol adhesive, zirconium balls and deionized water after grinding, and performing ball milling for 7 hours on a planetary ball mill;
s4: shaping and plastic discharge
The material obtained after ball milling is sieved by a 300-mesh sieve. And then placing the slurry in a centrifugal granulation dryer to prepare powder with fluidity, molding the obtained powder under the pressure of 8-10MPa by using molds with the diameters of 15mm and 65mm, and placing the molded blank in a cold isostatic press to apply the uniform hydraulic pressure of 200 MPa. Then placing the blank body in a high-temperature glue discharging furnace, heating to 800 ℃ at the speed of 2-5 ℃/min, preserving the temperature for 30min, and discharging organic matters;
s5: sintering
The blank body is embedded and sintered by adopting an inverted crucible, the temperature is raised to 1300-1350 ℃ at the speed of 3-6 ℃/min in a box type sintering furnace, the temperature is preserved for 3 hours, the blank body is sintered into porcelain, and then the porcelain is cooled along with the box. The diameter of the sintered ceramic piezoelectric ceramics with two specifications is 15mm for testing the piezoelectric performance, and the diameter of the sintered ceramic piezoelectric ceramics with two specifications is 65mm for testing the electrical performance of the drum-type transducer.
S6: slicing
The sintered piezoelectric ceramic with the diameter of 65mm is placed on a wire cutting machine to be cut into sheets with the diameter of 0.2 mm.
S7: silver firing
And (3) polishing two surfaces of the sintered piezoelectric ceramic smoothly, smearing electronic conductive silver paste on the surface of the piezoelectric ceramic by using a vertical screen printer, and then putting the piezoelectric ceramic into an electrothermal blowing drying oven for drying. Putting the piezoelectric ceramic piece into a high-temperature silver burning furnace, heating to 750-800 ℃, preserving heat for 20min, and cooling along with the furnace;
s8: polarization of
Putting the piezoelectric ceramic piece after silver burning into high-temperature silicone oil, and polarizing under the conditions that the polarizing temperature is 70-120 ℃, the polarizing time is 5-25min, and the polarizing voltage is 2.75kV/mm-3.75 kV/mm;
s8: testing piezoelectric performance
And (3) placing the polarized piezoelectric ceramic standard sheet with the diameter of 15mm for 24 hours at normal temperature, and testing the piezoelectric performance, XRD (X-ray diffraction) pattern, SEM (scanning Electron microscope) image and dielectric temperature pattern.
S9, preparing a drum-type piezoelectric transducer to test the road fatigue performance of the transducer
And bonding the polarized 65mm piezoelectric ceramic plate and the 304 stainless steel sheet by using structural adhesive, and putting the piezoelectric ceramic plate and the 304 stainless steel sheet into an electric heating air blowing drying box for curing for 5 hours at 75 degrees. The prepared drum-type piezoelectric transducer is put into a three-channel fatigue testing machine to test the fatigue performance of the drum-type piezoelectric transducer.
The invention also aims to provide a piezoelectric ceramic adaptive to the road vibration energy harvesting technology, which is prepared by the preparation method of the piezoelectric ceramic adaptive to the road vibration energy harvesting technology.
In addition, the invention also provides application of the piezoelectric ceramic adaptive to the road vibration energy harvesting technology in the technical field of road energy collection and utilization, which is prepared by a preparation method of the piezoelectric ceramic adaptive to the road vibration energy harvesting technology.
The invention has the beneficial effects that:
(1) The vibration energy harvesting technology based on the piezoelectric effect has the advantages of high power-electricity conversion efficiency, simple structure, no electromagnetic interference and the like, can supply power for the monitoring equipment of the traffic infrastructure, solves the problems of difficult power supply, difficult wiring and difficult transmission of the low-medium power consumption wireless sensor, and realizes the full-life cycle monitoring of the traffic infrastructure in a complex service environment.
(2) The invention provides a piezoelectric ceramic formula which is highly matched with road energy harvesting application, and the piezoelectric ceramic piece with excellent performance under the road vibration coupling action is obtained through material preparation, pre-burning, secondary ball milling, molding, plastic removal, sintering, slicing, silver burning and polarization, so that the optimal piezoelectric charge constant d33=857Pc/N under the condition of road piezoelectric material Curie temperature is successfully realized.
(3) The formula is subjected to surface mounting and curing to prepare the drum-type piezoelectric transducer, the drum-type piezoelectric transducer is placed in a three-channel fatigue testing machine, the drum-type piezoelectric transducer is continuously loaded for 60 hours at normal temperature under the conditions that the displacement is 0.5mm and the frequency is 10Hz, the open-circuit piezoelectric degradation rate is only 0.86 percent, the drum-type piezoelectric transducer has long-term stability of road power generation, and a good foundation is laid for the development of a road piezoelectric energy harvesting technology.
Drawings
FIG. 1 is a schematic structural diagram of a self-powered road vibration energy harvesting system according to an embodiment of the present invention;
FIG. 2 is a schematic flow diagram of a process for preparing a piezoelectric ceramic formulation suitable for road vibration energy harvesting technology in accordance with an embodiment of the present invention;
FIG. 3 is an XRD spectrum of a piezoelectric ceramic prepared to adapt to a road vibration energy harvesting technology in an embodiment of the invention;
FIG. 4 is an SEM image of a piezoelectric ceramic prepared to adapt to a road vibration energy harvesting technique in an embodiment of the present invention;
FIG. 5 is a dielectric temperature map of a piezoelectric ceramic fabricated to adapt to road vibration energy harvesting techniques in accordance with an embodiment of the present invention;
FIG. 6 is a graph of open-circuit voltage waveforms of a piezoelectric ceramic drum transducer prepared to adapt to a road vibration energy harvesting technology in an embodiment of the invention.
Reference numerals: 1. a repeater; 2. a wireless network; 3. a data processing center; 4. a piezoelectric transducer; 5. an energy storage device; 6. a traffic accessory device; 7. an asphalt concrete surface course; 8. a cement gravel stabilizing layer; 9. a gravel cushion layer; 10. an electronic precision balance; 11. a planetary ball mill; 12. a high-temperature box type sintering furnace; 13. a centrifugal granulation dryer; 14. an electric tablet press; 15. a cold isostatic press; 16. a wire cutting machine; 17. a vertical screen printer; 18. a withstand voltage tester; 19. PSN-PZT piezoelectric ceramics; 20. testing simulation software; 21. a servo motor controller; 22. a Tak oscilloscope; 23. a three-channel fatigue testing machine; 24. a drum piezoelectric transducer unit.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the embodiments, structures, characteristics and effects according to the present invention will be made with reference to the accompanying drawings and preferred embodiments.
A piezoelectric ceramic formula suitable for road energy harvesting technology mainly comprises a main component and an additional component, wherein the main component is Pb x Sr y Ba 1-x-y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1-z O 3 Wherein: 0.7. Ltoreq. X.ltoreq.0.75, 0.02. Ltoreq. Y.ltoreq.0.06, 0.95. Ltoreq. Z.ltoreq.0.98, an additional component 0.2wt.% of CaCO based on the mass of the main component 3 And 0.05wt% CdCO 3 The main component comprises Pb 3 O 4 ，TiO 2 ，ZrO 2 ，BaCO 3 ，SrCO 3 ，Sb 2 O 3 And Nb 2 O 5 Said Pb being 3 O 4 ，TiO 2 ，ZrO 2 ，BaCO 3 ，SrCO 3 ，Sb 2 O 3 And Nb 2 O 5 ，CaCO 3 ，CdCO 3 For analytical purification.
Example 1:
referring to fig. 2 to 5, a method for preparing a piezoelectric ceramic formulation adapted to a road energy harvesting technology,
s1: compounding according to the chemical formula Pb x Sr y Ba 1-x-y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1-z O 3 Separately placing lead tetraoxide, titanium dioxide, barium dioxide, strontium carbonate, barium carbonate, antimony trioxide, niobium pentoxide, calcium carbonate and barium carbonate in an electrothermal blowing dry box, drying at 120-150 deg.C for 7 hr, and mixing with 0.2wt% CaCO 3 And 0.05wt% CdCO 3 Weighing and uniformly mixing, placing the raw materials in a planetary ball mill for ball milling for 7 hours, and then drying the raw materials;
s2: pre-sintering, namely placing the mixed powder into an alumina crucible, covering and sealing the alumina crucible, placing the alumina crucible into a high-temperature pre-sintering furnace for pre-sintering, and synthesizing for 2.5 hours after heating to 960-1000 ℃;
s3: secondary ball milling
Grinding the block powder after pre-sintering, adding 10% polyvinyl alcohol adhesive, zirconium balls and deionized water after grinding, and performing ball milling for 7 hours on a planetary ball mill;
s4: shaping of
Filtering the ball-milled material through a 300-mesh screen, placing the slurry in a centrifugal granulation dryer to prepare flowable powder, dividing the obtained powder into two parts, wherein one part is molded by a die with the diameter of 15mm and the other part is molded by a die with the diameter of 65mm under the pressure of 8-10MPa, and placing the molded blank in a cold isostatic press to apply the uniform hydraulic pressure of 200 MPa.
S5: plastic row
And (3) placing the blank body in a high-temperature glue discharging furnace, heating to 800 ℃ at the speed of 2-5 ℃/min, preserving heat for 30min, and discharging organic matters.
S6: sintering
The method comprises the steps of embedding and sintering a blank body with the diameter of 15mm and a blank body with the diameter of 65mm in an inverted crucible, heating the blank body to 1300-1350 ℃ at the speed of 3-6 ℃/min in a box type sintering furnace, preserving heat for 3 hours, sintering the blank body into ceramic, cooling the ceramic along with the box, and using the piezoelectric ceramic with the diameter of 15mm as a piezoelectric performance test and using the piezoelectric ceramic with the diameter of 65mm as a drum type transducer as an electrical performance test.
S7: slicing
Placing the sintered piezoelectric ceramics with the diameter of 65mm on a wire cutting machine to cut into sheets with the diameter of 0.2 mm;
s8: silver firing
Polishing two surfaces of the sintered piezoelectric ceramic smoothly, smearing electronic conductive silver paste on the surface of the piezoelectric ceramic by using a vertical screen printer, then putting the piezoelectric ceramic into an electric heating blast drying box for drying, placing the piezoelectric ceramic into a high-temperature silver burning furnace, heating to 750-800 ℃, preserving the heat for 20min, and cooling along with the furnace;
s9: polarization of
And (3) putting the piezoelectric ceramic piece after silver burning into high-temperature silicone oil, and polarizing under the conditions that the polarizing temperature is 70-120 ℃, the polarizing time is 5-25min, and the polarizing voltage is 2.75kV/mm-3.75 kV/mm.
S10: testing piezoelectric performance
And (3) placing the polarized piezoelectric ceramic standard sheet with the diameter of 15mm for 24 hours at normal temperature, testing the piezoelectric performance of the piezoelectric ceramic standard sheet, and testing an XRD (X-ray diffraction) pattern, an SEM (scanning Electron microscope) image and a medium temperature pattern of the sintered ceramic.
S11: preparation of drum-type piezoelectric transducer for testing road fatigue performance
And bonding the polarized 65 mm-diameter piezoelectric ceramic plate and the 304 stainless steel sheet by using a structural adhesive, placing the bonded piezoelectric ceramic plate and the 304 stainless steel sheet into an electric heating air blowing drying oven for curing for 5 hours at 75 ℃, and placing the prepared drum-type piezoelectric transducer into a three-channel fatigue testing machine for testing the fatigue performance.
The main component is Pb x Sr y Ba 1-x-y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1-z O 3 Wherein: x =0.74; y =0.05; z =0.98 of the total mass of the steel,
TABLE I is a piezoelectric property test chart of example 1
The piezoelectric ceramic adaptive to the road vibration energy harvesting technology obtained by the preparation method of the embodiment 1 has excellent piezoelectric performance and dielectric performance. The polarization of the piezoelectric ceramic has larger dependence on temperature, the optimal piezoelectric voltage constant 855pC/N, the relative dielectric constant 3405, the electromechanical coupling coefficient 0.76, the mechanical quality factor 34.67, the dielectric loss 2.85 percent and better low-temperature polarization performance at 70 ℃, thereby providing a new idea for mass production of the ceramic and greatly improving the polarization process efficiency. The polarization time parameter of the piezoelectric ceramic has an optimal value, and the piezoelectric ceramic has an optimal piezoelectric voltage constant 857pC/N, a relative dielectric constant 3396, an electromechanical coupling coefficient of 0.79, a mechanical quality factor of 33.9 and dielectric loss of 2.95 percent at 15 min. With the increase of the polarization electric field, d33, kp and Qm of the piezoelectric ceramic are increased, and the piezoelectric ceramic has an optimal piezoelectric voltage constant 857pC/N, a relative dielectric constant 3405, an electromechanical coupling coefficient of 0.76, a mechanical quality factor of 38.01 and a dielectric loss of 2.85 percent.
The second embodiment is different from the first embodiment in that:
the main component is Pb x Sr y Ba 1-x-y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1-z O 3 Wherein: x =0.74; y =0.05; z =0.99 of the total weight of the composition,
TABLE II shows the piezoelectric property test chart of example 2
The piezoelectric ceramic adaptive to the road vibration energy harvesting technology obtained by the preparation method of the embodiment 2 has excellent piezoelectric performance and dielectric performance. The piezoelectric ceramic polarization has larger dependence on temperature, has an optimal piezoelectric voltage constant 695pC/N, a relative dielectric constant 3103, an electromechanical coupling coefficient of 0.58, a mechanical quality factor of 39.05 at 70 ℃, dielectric loss of 1.96 percent and excellent low-temperature polarization performance, provides a new idea for ceramic mass production, and greatly improves the polarization process efficiency. The polarization time parameter of the piezoelectric ceramic has an optimal value, and the optimal piezoelectric voltage constant 703pC/N, the relative dielectric constant 3099, the electromechanical coupling coefficient 0.62, the mechanical quality factor 38.185 and the dielectric loss 1.84 percent are obtained at 15 min. With the increase of the polarization electric field, d33, kp and Qm of the piezoelectric ceramic are increased, and the piezoelectric ceramic has an optimal piezoelectric voltage constant 704pC/N, a relative dielectric constant 2918, an electromechanical coupling coefficient of 0.54, a mechanical quality factor of 38.55 and a dielectric loss of 1.87 percent.
The third embodiment is different from the first and second embodiments in that:
the main component is Pb x Sr y Ba 1-x-y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1-z O 3 Wherein: x =0.74; y =0.05; z =0.97 of the total weight of the composition,
TABLE III shows the piezoelectric property test chart of example 3
The piezoelectric ceramic adaptive to the road vibration energy harvesting technology obtained by the preparation method of the embodiment 3 has excellent piezoelectric performance and dielectric performance. The polarization of the piezoelectric ceramics has larger dependence on temperature, the optimal piezoelectric voltage constant 730pC/N, the relative dielectric constant 3220, the electromechanical coupling coefficient 0.66, the mechanical quality factor 38.79 and the dielectric loss 2.13 percent at 70 ℃, and the low-temperature polarization performance is better, thereby providing a new idea for the mass production of ceramics and greatly improving the polarization process efficiency. The piezoelectric ceramic polarization time parameter has an optimal value, and has an optimal piezoelectric voltage constant 743pC/N, a relative dielectric constant 3216, an electromechanical coupling coefficient 0.68, a mechanical quality factor 37.951 and a dielectric loss 2.01% at 15 min. With the increase of the polarization electric field, d33, kp and Qm of the piezoelectric ceramic are increased, and the optimal piezoelectric voltage constant 745pC/N, the relative dielectric constant 3035, the electromechanical coupling coefficient 0.64, the mechanical quality factor 38.304 and the dielectric loss 2.04 percent exist.
Referring to fig. 1 and 6: the piezoelectric ceramic adaptive to the road vibration energy harvesting technology is prepared by a preparation method of the piezoelectric ceramic adaptive to the road vibration energy harvesting technology, and is solidified into a drum-type piezoelectric transducer through a patch, and the drum-type piezoelectric transducer is applied to road energy collection and utilization.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. The piezoelectric ceramic formula is characterized by mainly comprising main components and additional components, wherein the main components are as follows: pb x Sr y Ba 1-x-y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1-z O 3 Wherein: 0.7. Ltoreq. X.ltoreq.0.75, 0.02. Ltoreq. Y.ltoreq.0.06, 0.95. Ltoreq. Z.ltoreq.0.98, an additional component 0.2wt.% of CaCO based on the mass of the main component 3 And 0.05wt% CdCO 3 。
2. The piezoelectric ceramic formula adapted to the road energy harvesting technology according to claim 1, wherein: the main component is Pb 3 O 4 ，TiO 2 ，ZrO 2 ，BaCO 3 ，SrCO 3 ，Sb 2 O 3 And Nb 2 O 5 Said Pb 3 O 4 ，TiO 2 ，ZrO 2 ，BaCO 3 ，SrCO 3 ，Sb 2 O 3 And Nb 2 O 5 ，CaCO 3 ，CdCO 3 For analytical purification.
3. A method for preparing piezoelectric ceramics adapting to a road energy harvesting technology by adopting the piezoelectric ceramic formula adapting to the road energy harvesting technology of claim 2 is characterized by comprising the following steps:
s1: ingredients
According to the formula Pb x Sr y Ba 1-x-y (Zr 0.54 Ti 0.46 ) z (Sb 0.58 Nb 0.42 ) 1-z O 3 Separately placing lead tetraoxide, titanium dioxide, barium dioxide, strontium carbonate, barium carbonate, antimony trioxide, niobium pentoxide, calcium carbonate and barium carbonate in an electrothermal blowing dry box, drying at 120-150 deg.C for 7 hr, and mixing with 0.2wt% CaCO 3 And 0.05wt% CdCO 3 Weighing and uniformly mixing, placing the raw materials in a planetary ball mill for ball milling for 7 hours, and then drying the raw materials;
s2: pre-firing
Placing the mixed powder into an alumina crucible, covering and sealing, placing the alumina crucible into a high-temperature presintering furnace for presintering, and synthesizing for 2.5 hours after heating to 960-1000 ℃;
s3: secondary ball milling
Grinding the block powder after pre-sintering, adding 10% polyvinyl alcohol adhesive, zirconium balls and deionized water after grinding, and performing ball milling for 7 hours on a planetary ball mill;
s4: shaping of
Filtering the material obtained after ball milling through a 300-mesh screen, then placing the slurry in a centrifugal granulation dryer to prepare powder with fluidity, dividing the obtained powder into two parts, wherein one part is molded by a die with the diameter of 15mm and the other part is molded by a die with the diameter of 65mm under the pressure of 8-10MPa, and placing the molded blank in a cold isostatic press to apply uniform hydraulic pressure of 200 MPa.
S5: plastic row
And (3) placing the blank body in a high-temperature glue discharging furnace, heating to 800 ℃ at the speed of 2-5 ℃/min, preserving the temperature for 30min, and discharging organic matters.
S6: sintering
The method comprises the steps of embedding and sintering a blank body with the diameter of 15mm and a blank body with the diameter of 65mm in an inverted crucible, heating the blank body to 1300-1350 ℃ at the speed of 3-6 ℃/min in a box type sintering furnace, preserving heat for 3 hours, sintering the blank body into ceramic, cooling the ceramic along with the box, and using the piezoelectric ceramic with the diameter of 15mm as a piezoelectric performance test and using the piezoelectric ceramic with the diameter of 65mm as a drum type transducer as an electrical performance test.
S7: slicing
Placing the sintered piezoelectric ceramics with the diameter of 65mm on a wire cutting machine to cut into sheets with the diameter of 0.2 mm;
s8: silver firing
Polishing two surfaces of the sintered piezoelectric ceramic smoothly, smearing electronic conductive silver paste on the surface of the piezoelectric ceramic by using a vertical screen printer, then putting the piezoelectric ceramic into an electric heating blast drying box for drying, placing the piezoelectric ceramic into a high-temperature silver burning furnace, heating to 750-800 ℃, preserving the heat for 20min, and cooling along with the furnace;
s9: polarization of
And (3) putting the piezoelectric ceramic piece after silver burning into high-temperature silicone oil, and polarizing under the conditions that the polarizing temperature is 70-120 ℃, the polarizing time is 5-25min, and the polarizing voltage is 2.75kV/mm-3.75 kV/mm.
S10: testing piezoelectric performance
And (3) placing the polarized piezoelectric ceramic standard sheet with the diameter of 15mm for 24 hours at normal temperature, testing the piezoelectric performance of the piezoelectric ceramic standard sheet, and testing an XRD (X-ray diffraction) pattern, an SEM (scanning Electron microscope) image and a medium temperature pattern of the sintered ceramic.
S11: preparation of drum-type piezoelectric transducer for testing road fatigue performance
And bonding the polarized 65 mm-diameter piezoelectric ceramic plate and the 304 stainless steel sheet by using a structural adhesive, placing the bonded piezoelectric ceramic plate and the 304 stainless steel sheet into an electric heating air blowing drying oven for curing for 5 hours at 75 ℃, and placing the prepared drum-type piezoelectric transducer into a three-channel fatigue testing machine for testing the fatigue performance.
4. The piezoelectric ceramic adaptive to the road vibration energy harvesting technology is prepared by the preparation method of the piezoelectric ceramic adaptive to the road vibration energy harvesting technology according to claim 3.
5. The application of the piezoelectric ceramic adaptive to the road vibration energy harvesting technology prepared by the preparation method of the piezoelectric ceramic adaptive to the road vibration energy harvesting technology in the technical field of road energy collection and utilization is characterized in that the piezoelectric ceramic is prepared into a drum-type piezoelectric transducer by patch and solidification.
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| US20050085373A1 (en) * | 2003-10-15 | 2005-04-21 | De Liufu | Compositions for high power piezoelectric ceramics |
| US20060229187A1 (en) * | 2005-04-11 | 2006-10-12 | De Liufu | Compositions for high power piezoelectric ceramics |
| CN101265090A (en) * | 2008-04-21 | 2008-09-17 | 天津大学 | Strontium and barium doping lead niobium-stibium zirconate-titanate series piezoelectric ceramic and preparation method thereof |
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