CN114315345B - High-temperature piezoelectric energy collection ceramic material with wide-temperature stable transduction coefficient and preparation method thereof - Google Patents

High-temperature piezoelectric energy collection ceramic material with wide-temperature stable transduction coefficient and preparation method thereof Download PDF

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CN114315345B
CN114315345B CN202210028251.5A CN202210028251A CN114315345B CN 114315345 B CN114315345 B CN 114315345B CN 202210028251 A CN202210028251 A CN 202210028251A CN 114315345 B CN114315345 B CN 114315345B
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侯育冬
于肖乐
郑木鹏
朱满康
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Beijing University of Technology
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Abstract

A high-temperature piezoelectric energy collecting ceramic material with wide-temperature stable transduction coefficient and a preparation method thereof belong to the field of piezoelectric ceramic materials. The chemical composition of the matrix of the ceramic material is zBiScO 3 ‑yBi(Zn 2/3 Ta 1/3 )O 3 ‑xPbTiO 3 (0.605. Ltoreq. X.ltoreq.0.64, 0.005. Ltoreq. Y.ltoreq.0.03, z = 1-x-y). The preparation method adopts a high-temperature solid phase method, and comprises the steps of weighing corresponding raw materials according to a stoichiometric ratio, and then sequentially carrying out wet grinding, drying, calcining, granulating, compression molding and sintering. The high-temperature piezoelectric ceramic material provided by the invention has high and thermally stable transduction coefficients in a wide temperature region, is beneficial to enhancing the working stability of a high-temperature piezoelectric energy collecting device, and has remarkable social significance and application value.

Description

High-temperature piezoelectric energy collection ceramic material with wide-temperature stable transduction coefficient and preparation method thereof
Technical Field
The invention belongs to the field of piezoelectric ceramic materials, and particularly relates to a piezoelectric ceramic material with high and temperature-stable transduction coefficient for high-temperature piezoelectric energy collection in a wide temperature range and a preparation method thereof.
Background
The development of advanced fields such as aerospace, nuclear energy conversion, unmanned driving and the like remarkably promotes the progress of human beings. Meanwhile, a large number of wireless sensors are put into the fields to perform structural health monitoring, data acquisition and transmission and the like, so that the running state of equipment is fed back in real time, and the safety of the equipment is ensured. The micro-sensor in these fields operates at temperatures not less than 200 ℃ and even up to 300 ℃, which presents a great challenge to the way of supplying electric energy. The existing power supply mode mainly uses a battery, but the power supply requirement is difficult to meet due to inherent defects of limited service life, no high temperature resistance and the like. The piezoelectric energy collector can capture waste vibration energy widely existing in the environment to realize clean power generation based on the positive piezoelectric effect of piezoelectric ceramics, and is a very promising electromechanical conversion device for long-term power supply of the wireless sensor.
At present, pb (Zr, ti) O is dominant in the piezoelectric market 3 The perovskite-based piezoelectric material has high piezoelectric activity, but the Curie temperature is not more than 386 ℃, the safe use temperature is limited to 200 ℃, the piezoelectric property is seriously deteriorated due to depolarization caused by overhigh temperature, and the application of the perovskite-based piezoelectric material in the high-temperature field is seriously limited. And BiScO of perovskite structure 3 -PbTiO 3 Material for having a high dwellingThe internal temperature and the high-voltage electrical activity become main research systems in the field of high-temperature piezoelectricity.
For a high-temperature piezoelectric energy collecting material with high electromechanical conversion capacity, the high-temperature piezoelectric energy collecting material not only has a high Curie temperature, but also has a high energy density (u). The energy density (u) is expressed as:
Figure BDA0003465264530000011
wherein d and g are the transduction coefficient of the piezoelectric ceramic, A is the stress area of the piezoelectric ceramic, and F is the external exciting force. As can be seen from equation (1), the transduction coefficient dominates the energy density of the energy harvesting material.
In addition, considering that the high-temperature piezoelectric energy collector also faces the impact of temperature change in the practical application process, the transduction coefficient of the piezoelectric material is kept stable (the fluctuation rate (eta) is less than or equal to +/-15%) in a wide temperature range (25-300 ℃), and the safe and reliable operation of the device is favorably ensured. Therefore, the temperature stability of the transduction coefficient of the high-temperature piezoelectric energy collecting material was evaluated on the basis of 200 ℃, and the temperature fluctuation ratio (η) of the transduction coefficient (d · g) was expressed as:
Figure BDA0003465264530000021
wherein, (d.g) T Is the transduction coefficient of the material at a certain test temperature, (d.g) 200℃ The transduction coefficient of the material at 200 ℃.
In the invention, biScO is used 3 -PbTiO 3 (BS-PT for short) as matrix, and introducing Bi (Zn) 2/3 Ta 1/3 )O 3 Primitive, construct zBiScO 3 -yBi(Zn 2/3 Ta 1/3 )O 3 -xPbTiO 3 (abbreviated as zBS-yBZT-xPT) ternary high-temperature piezoelectric ceramic material system. Among them, the best BS-BZT-PT sample not only has high Curie temperature, but also has high and temperature stable transduction coefficient (d) at 25-300 DEG C 33 ·g 33 =12481×10 -15 m 2 N, eta less than or equal to +/-15%), yuyuan-youIn patent CN 107698252A, 0.36BS-0.64PT piezoelectric material. So far, the excellent transduction coefficient and temperature stability materials of the system are not reported.
Disclosure of Invention
The invention is characterized in that Sc ions in a BS-PT matrix are replaced by the combination of Zn and Ta composite ions with strong ferroelectricity activity and large element mass, and the combination is based on metastable Bi (Zn) 2/3 Ta 1/3 )O 3 The elements have high squareness, so that the displacement amplitude of B-site ions in the perovskite oxygen octahedron and the temperature stability of a phase structure are enhanced, and a multiple phase boundary design theory is combined, so that the high Curie temperature, high thermal stability and transduction coefficient are obtained.
The invention aims to obtain a high-temperature piezoelectric material zBS-yBZT-xPT with high Curie temperature, high temperature and stable transduction coefficient, thereby laying a solid material foundation for preparing a high-temperature piezoelectric energy collector with excellent electromechanical conversion capability in a wide temperature region.
The material of the invention is characterized in that zBiScO 3 -yBi(Zn 2/3 Ta 1/3 )O 3 -xPbTiO 3 (zBS-yBZT-xPT) wherein x is more than or equal to 0.605 and less than or equal to 0.64, y is more than or equal to 0.005 and less than or equal to 0.03, and z is 1-x-y. Preferably x =0.620, x =0.01, z =0.37, i.e. 0.37BS-0.01BZT-0.620PT, the sample having a transduction coefficient d at 200 ℃ 33 ·g 33 =12481×10 -15 m 2 and/N, the fluctuation rate eta is less than or equal to +/-15% at the temperature of 25-300 ℃, and the method can be used for preparing advanced high-temperature piezoelectric energy collecting devices.
The preparation method of the high-temperature piezoceramic material with high and thermally stable transduction coefficients in the ultra-wide temperature region is characterized by being prepared by a high-temperature solid phase method, and specifically comprises the following steps:
(1) According to zBiScO 3 -yBi(Zn 2/3 Ta 1/3 )O 3 -xPbTiO 3 (x is more than or equal to 0.605 and less than or equal to 0.64, y is more than or equal to 0.005 and less than or equal to 0.03, and z is not less than 1-x-y) the stoichiometric ratio of the elements in the piezoceramic material is respectively weighed 2 O 3 、Sc 2 O 3 、ZnO、Ta 2 O 5 、Pb 3 O 4 、TiO 2 Six raw materials are weighedPutting the good raw materials into a ball milling tank, putting the ball milling tank into a horizontal ball mill by taking absolute ethyl alcohol as a medium, carrying out ball milling for 24 hours, and then putting the obtained mixture into an oven at 100 ℃ for drying;
(2) Grinding the dried mixture, placing the ground mixture into an alumina crucible, calcining the mixture at 800 ℃, preserving heat for 2 hours, and cooling the mixture to room temperature along with a furnace;
(3) Pouring the calcined powder into a ball milling tank, and adding absolute ethyl alcohol for secondary ball milling for 24 hours;
(4) Adding a binder into the powder obtained by secondary ball milling, granulating, sieving, pressing under pressure to prepare a ceramic biscuit, and heating for removing gel;
if polyvinyl alcohol (PVA) binder with the mass fraction of 5wt.% is added, the pressure is maintained for 2min under the uniaxial pressure of 100MPa, the mixture is pressed into ceramic biscuit, then the glue discharging treatment is carried out at 560 ℃, the heat preservation is carried out for 3h, and the mixture is cooled to the room temperature along with the furnace;
(5) Sintering the biscuit body subjected to the binder removal treatment at 1050-1150 ℃, preserving heat for 2h, and cooling to room temperature along with the furnace; preferably 1150 deg.c.
And (3) carrying out surface polishing treatment on the sintered ceramic sample, sintering and infiltrating a silver electrode, and then placing the ceramic sample in 120 ℃ silicon oil to polarize for 30min at a voltage of 4 kV/mm. And after aging for 24 hours at room temperature, testing the electrical property of the ceramic sample.
Wherein, the optimal ceramic sample composition for obtaining the pure perovskite structure is x =0.620, x =0.01, z =0.37, namely 0.37BS-0.01BZT-0.620PT. Through in-situ temperature change test, the sample has an energy conversion coefficient d at 200 DEG C 33 ·g 33 =12481×10 -15 m 2 The fluctuation rate eta is less than or equal to +/-15 percent at the temperature of between 25 and 300 ℃, and the application requirement of the high-temperature piezoelectric energy collector can be met.
Compared with the prior art, the invention has the following advantages:
(1) The optimal sample in the invention has high Curie temperature and high transduction coefficient, is favorable for enhancing the electromechanical transformation capacity of the high-temperature piezoelectric energy collector, and is a ceramic material for collecting high-temperature piezoelectric energy with high competitiveness.
(2) The optimal sample transduction coefficient has excellent temperature stability in an ultra-wide temperature region of 25-300 ℃, is favorable for enhancing the working temperature reliability of devices, and is a high-temperature piezoelectric energy collecting ceramic material with great potential for wide-temperature application.
Drawings
FIG. 1 is an XRD spectrum of ceramic materials 0.365BS-0.005BZT-0.630PT (0.5-630 for short), 0.37BS-0.01BZT-0.620PT (1-620 for short), 0.36BS-0.02BZT-0.620PT (2-620 for short) and 0.355BS-0.03BZT-0.615PT (3-615 for short) in the practice of the present invention.
FIG. 2 is a graph showing the in-situ temperature-varying transduction coefficients (d) of 0.365BS-0.005BZT-0.630PT (0.5-630 for short) 0.37BS-0.01BZT-0.620PT (1-620 for short), 0.36BS-0.02BZT-0.620PT (2-620 for short) and 0.355BS-0.03BZT-0.615PT (3-615 for short) ceramic materials in accordance with the practice of the present invention 33 ·g 33 ) The test frequency was 100Hz.
FIG. 3 is a graph showing the temperature fluctuation coefficient (η) of the in-situ temperature-varying transduction coefficient of ceramic materials 0.365BS-0.005BZT-0.630PT (0.5-630 for short) 0.37BS-0.01BZT-0.620PT (1-620 for short), 0.36BS-0.02BZT-0.620PT (2-620 for short) and 0.355BS-0.03BZT-0.615PT (3-615 for short) in accordance with the present invention, wherein d is 200 ℃ 33 ·g 33 For reference, the temperature stability of the high temperature piezoelectric energy harvesting ceramic material was evaluated.
Detailed Description
The present invention will be described in detail below by way of examples, which are for illustrative purposes only and are not intended to limit the present invention.
The invention provides a high-temperature piezoelectric energy collection ceramic material with a wide-temperature stable transduction coefficient, which is characterized by comprising the chemical composition of zBiScO 3 -yBi(Zn 2/3 Ta 1/3 )O 3 -xPbTiO 3 (0.605. Ltoreq. X.ltoreq.0.64, 0.005. Ltoreq. Y.ltoreq.0.03, z = 1-x-y). The raw materials of the composition comprise: bi 2 O 3 、Sc 2 O 3 、ZnO、Ta 2 O 5 、Pb 3 O 4 And TiO 2 2 . The preparation method comprises the following steps: firstly, weighing raw materials according to the stoichiometric ratio of each component, then putting the raw materials into a ball milling tank, taking absolute ethyl alcohol as a medium, carrying out ball milling for 24 hours, and then carrying out ball milling on the raw materialsDrying the obtained mixture in a drying oven at 100 ℃; grinding the dried mixture, putting the ground mixture into a closed alumina crucible, calcining the mixture at 800 ℃, preserving heat for 2 hours, and cooling the mixture to room temperature along with a furnace; placing the calcined product and ball milling medium absolute ethyl alcohol into a ball milling tank for secondary ball milling for 24 hours, and drying ball milling slurry at 100 ℃; adding a binder with the mass fraction of about 5wt.% into the dried powder, granulating, sieving, pressing into a ceramic biscuit, discharging the glue, sintering at 1150 ℃, preserving the heat for 2h, and cooling to room temperature along with the furnace. And (3) polishing the surface of the sintered ceramic sample, sintering and infiltrating a silver electrode, and then placing the ceramic sample in silicone oil at 120 ℃ to polarize for 30min at a voltage of 4 kV/mm. And after aging for 24 hours at room temperature, testing the electrical property of the ceramic sample.
The following examples further illustrate the substantial features and significant advantages of the present invention. It should be noted that the invention is in no way limited to the embodiments presented.
Example 1:
bi is weighed according to the chemical formula of 0.365BS-0.005BZT-0.630PT (0.5-630 for short) 2 O 3 、Sc 2 O 3 、ZnO、Ta 2 O 5 、Pb 3 O 4 And TiO 2 And ball milling is carried out for 24 hours by taking absolute ethyl alcohol as a medium. The mixture is calcined for 2 hours at 800 ℃ after being dried at 100 ℃; and adding absolute ethyl alcohol, performing secondary ball milling for 24 hours, adding a binder with the mass fraction of about 5wt.% into the dried powder, granulating, sieving, pressing into a ceramic biscuit, performing binder removal treatment, sintering at 1150 ℃, preserving heat for 2 hours, and cooling to room temperature along with the furnace. And (3) polishing the surface of the sintered ceramic sample, sintering and infiltrating a silver electrode, and then placing the ceramic sample in silicone oil at 120 ℃ to polarize for 30min at a voltage of 4 kV/mm. And after aging for 24 hours at room temperature, testing the electrical property of the ceramic sample.
Example 2:
the ceramic material 0.37BS-0.01BZT-0.620PT (1-620) was prepared in the same manner as in example 1.
Example 3:
the ceramic material 0.36BS-0.02BZT-0.620PT (2-620) was prepared in the same manner as in example 1.
Example 4
The ceramic material 0.355BS-0.03BZT-0.615PT (3-615 for short) was prepared in the same manner as in example 1.
Table 1 comparative table of properties of the above examples
Figure BDA0003465264530000061

Claims (5)

1. A high-temperature piezoelectric energy collection ceramic material with a wide-temperature stable transduction coefficient is characterized in that the chemical composition general formula is as follows: zBiScO 3 -yBi(Zn 2/3 Ta 1/3 )O 3 -xPbTiO 3 ,0.605≤x≤0.64,0.005≤y≤0.03,z=1-x-y。
2. The high temperature piezoelectric energy harvesting ceramic material having a broad temperature stability transduction coefficient according to claim 1, wherein x is 0.620, y is 0.01, and z is 0.37.
3. A high temperature piezoelectric energy harvesting ceramic material having a wide temperature range stable transduction coefficient according to claim 1, wherein x =0.620, y =0.01, z =0.37 ceramic sample has a high curie temperature 441 ℃ with a transduction coefficient d of 200 ℃ 33 ·g 33 =12481×10 -15 m 2 the/N is taken as a reference, and the fluctuation rate (eta) of the transduction coefficient is not more than +/-15% at the temperature of 25-300 ℃.
4. A method for the preparation of a ceramic material according to any of claims 1-3, characterized in that it is prepared according to the following steps:
(1) Raw material Bi 2 O 3 、Sc 2 O 3 、ZnO、Ta 2 O 5 、Pb 3 O 4 And TiO 2 Weighing the piezoelectric ceramic material according to the stoichiometric ratio of elements, putting the weighed raw materials into a ball milling tank, putting the raw materials into a horizontal ball mill by taking absolute ethyl alcohol as a medium, carrying out ball milling for 24 hours, and then putting the obtained mixture into an oven at 100 ℃ for drying;
(2) Grinding the dried mixture, placing the ground mixture into an alumina crucible, calcining the mixture at 800 ℃, preserving heat for 2 hours, and cooling the mixture to room temperature along with a furnace;
(3) Pouring the calcined powder into a ball milling tank, adding absolute ethyl alcohol for secondary ball milling for 24 hours, and then placing the obtained mixture into an oven at 100 ℃ for drying;
(4) Adding a binder into the dried powder, granulating, sieving, pressing under pressure to prepare a ceramic biscuit, and heating for removing glue;
(5) Sintering the biscuit body subjected to the binder removal treatment at 1150 ℃, preserving heat for 2 hours, and cooling to room temperature along with the furnace;
(6) And polishing the prepared ceramic wafer, sintering and infiltrating a silver electrode, and artificially polarizing to obtain the piezoelectric ceramic material.
5. Use of a ceramic material according to any of claims 1-3 for a piezoelectric energy harvester.
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