CN111900246A - Polarization method of lithium-sodium niobate-based leadless piezoelectric ceramic - Google Patents
Polarization method of lithium-sodium niobate-based leadless piezoelectric ceramic Download PDFInfo
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- CN111900246A CN111900246A CN202010782897.3A CN202010782897A CN111900246A CN 111900246 A CN111900246 A CN 111900246A CN 202010782897 A CN202010782897 A CN 202010782897A CN 111900246 A CN111900246 A CN 111900246A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- 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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Abstract
The invention discloses a polarization method of lithium-sodium niobate-based lead-free piezoelectric ceramics, which is mainly divided into first polarization and second polarization; putting the lithium sodium niobate leadless piezoelectric ceramic into silicone oil, heating to a set temperature, keeping for a certain time under a set polarizing electric field intensity, and carrying out first polarization; and then cooling, taking out the ceramic sample, standing, then putting the ceramic sample into silicon oil again, heating, keeping for a certain time under the set polarizing electric field intensity, carrying out second polarization, finally cooling, taking out and removing surface silicon oil, and testing the piezoelectric property at room temperature (25 ℃), wherein experiments show that the piezoelectric constant can be increased from 60pC/N to 115pC/N of common polarization. The method reasonably selects the polarization condition, and improves the piezoelectric performance by controlling the size and the duration of a polarization electric field between electrodes of the piezoelectric ceramic sample during polarization as well as the environment and the temperature of the sample; by using the polarization method, the lithium-sodium niobate-based lead-free piezoelectric ceramic has excellent piezoelectric performance.
Description
Technical Field
The invention relates to polarization of a lead-free piezoelectric ceramic material, in particular to a polarization method of a lithium sodium niobate-based lead-free piezoelectric ceramic.
Background
Piezoelectric materials have found widespread use in industry due to their ability to convert mechanical and electrical energy. Piezoelectric materials are used as sensors, actuators and transducers, for example: lens auto focus, microphone, headphone, and sonar. Since lead-based piezoelectric ceramics were invented in the early days, for example, lead zirconate titanate (PZT) -based ceramics, have been the first choice for commercial product material design. However, lead element has proved to be a serious hazard to human health and ecological environment, so that a demand for using an environmentally friendly lead-free piezoelectric material is raised in many countries of the world. For example, the directive about the restriction of the use of certain harmful components in electronic and electrical devices (RoHS), proposed by the european union in 2006, mentions the content of the pre-elements in the specification of electronic and electrical devices. Accordingly, scientists have invested great efforts in developing lead-free piezoelectric ceramics to replace lead-based piezoelectric ceramics.
In 2004, Kimura et al found that the mechanical quality factor Qm of the lithium sodium niobate-based lead-free piezoelectric ceramic after heat treatment reached 3000, which made the lithium sodium niobate-based lead-free piezoelectric ceramic have a competitive power in application of high power devices compared with lead-free piezoelectric ceramic of other components, and then received a great deal of attention. However, compared with the existing lead-free piezoelectric ceramics, the lithium sodium niobate-based lead-free piezoelectric ceramics has higher coercive field and lower piezoelectric constant. Therefore, it is more difficult to impart polarization to the macroscopic piezoelectric properties, and the lower piezoelectric constant also affects the application value.
Disclosure of Invention
The invention aims to provide a method for polarizing lithium-sodium niobate-based lead-free piezoelectric ceramics aiming at the defects in the prior art, so that the lithium-sodium niobate-based lead-free piezoelectric ceramics are sufficiently polarized, the piezoelectric performance of the lithium-sodium niobate-based lead-free piezoelectric ceramics is improved, and the application value of the lithium-sodium niobate-based lead-free piezoelectric ceramics is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a polarization method of lithium-sodium niobate-based lead-free piezoelectric ceramics mainly comprises first polarization and second polarization, and specifically comprises the following steps:
s1: preparing before polarization, putting the lithium-sodium niobate-based lead-free piezoelectric ceramic into silicone oil, and heating;
s2: first polarization, namely polarizing for a set time under a set polarization electric field intensity, keeping the electric field intensity unchanged after finishing the polarization, and naturally cooling the silicone oil to 25 ℃;
s3: taking the lithium niobate sodium-based lead-free piezoelectric ceramic out of the silicone oil, and directly standing in the air;
s4: second polarization, putting the standing lithium niobate sodium-based lead-free piezoelectric ceramic into silicone oil again, and heating; polarizing for a set time under a set polarizing electric field intensity, and then naturally cooling to 25 ℃;
s5: and taking out the lithium niobate sodium-based lead-free piezoelectric ceramic after the second polarization from the silicone oil, removing the silicone oil on the surface of the lithium niobate sodium-based lead-free piezoelectric ceramic, standing for a set time, and measuring the piezoelectric property of the lithium niobate sodium-based lead-free piezoelectric ceramic by using a quasi-static piezoelectric coefficient tester to obtain a piezoelectric constant at 25 ℃.
Preferably, in step S1, the temperature of the silicone oil is raised to 80-120 ℃ at a rate of 10 ℃/min.
Preferably, in step S2, the polarization electric field strength is set to 3-5 kV/mm, and the polarization is maintained for 30-60 min.
Preferably, in step S3, the lithium sodium niobate-based lead-free piezoelectric ceramic is taken out from the silicone oil and then left in the air for 24 to 48 hours.
Preferably, in step S4, the temperature of the silicone oil is raised to 80-120 ℃ at a speed of 10 ℃/min, the intensity of the polarized electric field is set to 4-6 kV/mm, and the polarization is maintained for 30-60 min.
Preferably, in step S5, the silicone oil on the surface of the lithium sodium niobate-based lead-free piezoelectric ceramic is removed, and the piezoelectric property is measured after the lithium sodium niobate-based lead-free piezoelectric ceramic is left for 24 hours.
Preferably, the polarization directions of the lithium sodium niobate-based lead-free piezoelectric ceramics are kept consistent during the first polarization and the second polarization.
The invention has the beneficial effects that:
aiming at the lithium sodium niobate-based lead-free piezoelectric ceramics, the invention improves the piezoelectric performance by reasonably selecting the polarization condition, namely controlling the size and the duration of a polarization electric field between electrodes of a lithium sodium niobate-based lead-free piezoelectric ceramic sample during polarization, and the environment and the temperature of the sample. The invention adopts a twice polarization mode, the ceramic sample after the first polarization is kept stand in the air, and after a period of aging, the maximum polarization voltage of the ceramic sample can be improved under the condition of ensuring that the ceramic is not broken down during the second polarization, so that the residual polarization intensity is improved, and the rearrangement of the internal electric domains is more orderly. Therefore, the piezoelectric coefficient of the lithium-sodium niobate-based lead-free piezoelectric ceramic after twice polarization can be remarkably improved, and the piezoelectric constant of the lithium-sodium niobate-based lead-free piezoelectric ceramic is improved from 60pC/N of common polarization to 115pC/N at room temperature, namely 25 ℃ through tests.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are conventionally obtained commercially or prepared by conventional methods.
Example 1:
the polarization of the lithium-sodium niobate-based lead-free piezoelectric ceramic of the embodiment comprises the following steps:
s1: putting a lithium-sodium niobate-based lead-free piezoelectric ceramic sample into silicone oil, and heating the silicone oil to 120 ℃ at the speed of 10 ℃/min;
s2: setting the intensity of the polarized electric field to 5kV/mm, keeping the intensity of the polarized electric field for 30min, keeping the intensity of the electric field unchanged, and naturally cooling the silicone oil to room temperature (25 ℃);
s3: taking out the ceramic sample from the silicone oil, and placing the ceramic sample in the air for 48 hours;
s4: after standing, putting the ceramic sample into the silicone oil again, and heating the silicone oil to 120 ℃ at the speed of 10 ℃/min;
s5: setting the intensity of the polarized electric field to be 6kV/mm, keeping for 30min, and then naturally cooling to room temperature (25 ℃);
s6: and taking the sodium lithium niobate-based lead-free piezoelectric ceramic subjected to S5 out of the silicone oil, removing the surface silicone oil, standing for 24 hours, and measuring the piezoelectric property of the piezoelectric ceramic by using a quasi-static piezoelectric coefficient tester to obtain the piezoelectric constant of 113pC/N at room temperature.
Example 2:
the polarization of the lithium-sodium niobate-based lead-free piezoelectric ceramic of the embodiment comprises the following steps:
s1: putting a lithium-sodium niobate-based lead-free piezoelectric ceramic sample into silicone oil, and heating the silicone oil to 100 ℃ at the speed of 10 ℃/min;
s2: setting the intensity of the polarized electric field to 4kV/mm, keeping the intensity of the polarized electric field for 45min, keeping the intensity of the electric field unchanged, and naturally cooling the silicone oil to room temperature (25 ℃);
s3: taking out the ceramic sample from the silicone oil, and placing the ceramic sample in the air for 36 hours;
s4: after standing, putting the ceramic sample into the silicone oil again, and heating the silicone oil to 100 ℃ at the speed of 10 ℃/min;
s5: setting the intensity of the polarized electric field to 5kV/mm, keeping for 45min, and then naturally cooling to room temperature (25 ℃);
s6: and taking the sodium lithium niobate-based lead-free piezoelectric ceramic subjected to S5 out of the silicone oil, removing the surface silicone oil, standing for 24 hours, and measuring the piezoelectric property of the piezoelectric ceramic by using a quasi-static piezoelectric coefficient tester to obtain the piezoelectric constant of 115pC/N at room temperature.
Example 3:
the polarization of the lithium-sodium niobate-based lead-free piezoelectric ceramic of the embodiment comprises the following steps:
s1: putting a lithium-sodium niobate-based lead-free piezoelectric ceramic sample into silicone oil, and heating the silicone oil to 80 ℃ at the speed of 10 ℃/min;
s2: setting the intensity of the polarized electric field to be 3kV/mm, keeping the intensity of the polarized electric field for 60min, keeping the intensity of the electric field unchanged, and naturally cooling the silicone oil to room temperature (25 ℃);
s3: taking out the ceramic sample from the silicone oil, and placing the ceramic sample in the air for 24 hours;
s4: after standing, putting the ceramic sample into the silicone oil again, and heating the silicone oil to 80 ℃ at the speed of 10 ℃/min;
s5: setting the intensity of the polarized electric field to 4kV/mm, keeping for 60min, and then naturally cooling to room temperature (25 ℃);
s6: and (3) taking the sodium lithium niobate-based lead-free piezoelectric ceramic subjected to S5 out of the silicone oil, removing the surface silicone oil, standing for 24 hours, and measuring the piezoelectric property of the piezoelectric ceramic by using a quasi-static piezoelectric coefficient tester to obtain the piezoelectric ceramic with the piezoelectric constant of 111pC/N at room temperature.
It should be noted that:
1) in the embodiments 1 to 3, the lithium sodium niobate-based lead-free piezoelectric ceramic is placed in the silicone oil, so that the influence of air breakdown on the sample in the subsequent polarization process can be prevented, and the influence of the space charge effect on the sample can be reduced by increasing the temperature of the silicone oil;
2) in examples 1 to 3, after the first polarization, the ceramic sample is allowed to stand in the air for a period of time, so as to properly age the ceramic sample, and ensure that the maximum polarization voltage can be increased during the second polarization, thereby increasing the remanent polarization strength, and making the rearrangement of the internal electric domains more orderly, so that the piezoelectric performance of the lithium sodium niobate-based lead-free piezoelectric ceramic after the second polarization is significantly improved.
Comparative example:
in contrast to example 2, the polarization of the lithium sodium niobate-based lead-free piezoelectric ceramic of this comparative example was carried out according to the following procedure:
s1: putting the lithium-sodium niobate-based lead-free piezoelectric ceramic into silicone oil, and heating the silicone oil to 100 ℃ at the speed of 10 ℃/min;
s2: setting the intensity of the polarized electric field to 4kV/mm, keeping the intensity of the polarized electric field for 45min, keeping the intensity of the electric field unchanged, and naturally cooling the silicone oil to room temperature (25 ℃);
s3: and (3) removing the silicone oil on the surface, standing for 24h, and measuring the piezoelectric property of the material by using a quasi-static piezoelectric coefficient tester to obtain the material with the piezoelectric constant of 60pC/N at room temperature.
In conclusion, the polarization method of the invention adopts a mode of polarization twice by reasonably selecting polarization conditions, namely controlling the size and duration of a polarization electric field and controlling the environmental temperature of a sample, so that the final lithium-sodium niobate-based lead-free piezoelectric ceramic has excellent piezoelectric performance and higher application value.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A method for polarizing a lithium-sodium niobate-based lead-free piezoelectric ceramic is characterized by mainly comprising a first polarization and a second polarization, and specifically comprising the following steps:
s1: preparing before polarization, putting the lithium-sodium niobate-based lead-free piezoelectric ceramic into silicone oil, and heating;
s2: first polarization, namely polarizing for a set time under a set polarization electric field intensity, keeping the electric field intensity unchanged after finishing the polarization, and naturally cooling the silicone oil to 25 ℃;
s3: taking the lithium niobate sodium-based lead-free piezoelectric ceramic out of the silicone oil, and directly standing in the air;
s4: second polarization, putting the standing lithium niobate sodium-based lead-free piezoelectric ceramic into silicone oil again, and heating; polarizing for a set time under a set polarizing electric field intensity, and then naturally cooling to 25 ℃;
s5: and taking out the lithium niobate sodium-based lead-free piezoelectric ceramic after the second polarization from the silicone oil, removing the silicone oil on the surface of the lithium niobate sodium-based lead-free piezoelectric ceramic, standing for a set time, and measuring the piezoelectric property of the lithium niobate sodium-based lead-free piezoelectric ceramic by using a quasi-static piezoelectric coefficient tester to obtain a piezoelectric constant at 25 ℃.
2. The method for polarizing a lithium sodium niobate-based lead-free piezoelectric ceramic according to claim 1, wherein in step S1, the temperature of the silicone oil is raised to 80 to 120 ℃ at a rate of 10 ℃/min.
3. The method for poling a lithium sodium niobate-based lead-free piezoelectric ceramic according to claim 1, wherein in step S2, the poling electric field strength is set to 3 to 5kV/mm, and poling is maintained for 30 to 60 min.
4. The method for poling a lithium sodium niobate-based lead-free piezoelectric ceramic according to claim 1, wherein in step S3, the lithium sodium niobate-based lead-free piezoelectric ceramic is taken out from silicone oil and left in the air for 24 to 48 hours.
5. The method for poling a lithium sodium niobate-based lead-free piezoelectric ceramic according to claim 1, wherein in step S4, the temperature of the silicone oil is raised to 80 to 120 ℃ at a rate of 10 ℃/min, the intensity of the poling electric field is set to 4 to 6kV/mm, and poling is maintained for 30 to 60 min.
6. The method for poling lithium sodium niobate-based lead-free piezoelectric ceramic according to claim 1, wherein in step S5, the silicone oil on the surface of the lithium sodium niobate-based lead-free piezoelectric ceramic is removed, and the piezoelectric properties of the lithium sodium niobate-based lead-free piezoelectric ceramic are measured after the lithium sodium niobate-based lead-free piezoelectric ceramic is left for 24 hours.
7. The method for polarizing a lithium sodium niobate-based lead-free piezoelectric ceramic according to claim 1, wherein the polarization direction of the lithium sodium niobate-based lead-free piezoelectric ceramic is kept in agreement between the first polarization and the second polarization.
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Application publication date: 20201106 |