CN111463344A - Preparation method of piezoelectric single crystal element - Google Patents
Preparation method of piezoelectric single crystal element Download PDFInfo
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- CN111463344A CN111463344A CN201910059914.8A CN201910059914A CN111463344A CN 111463344 A CN111463344 A CN 111463344A CN 201910059914 A CN201910059914 A CN 201910059914A CN 111463344 A CN111463344 A CN 111463344A
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- H10N30/01—Manufacture or treatment
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- 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 present invention provides a method for manufacturing a piezoelectric single crystal element, comprising: preparing an annular piezoelectric single crystal material and coating a conductive electrode on the surface of the piezoelectric single crystal material; dividing and polarizing the piezoelectric single crystal material: firstly, uniformly dividing an annular piezoelectric single crystal material into a plurality of sector-shaped material blocks along the circumferential direction by taking the axis of the annular piezoelectric single crystal material as a center, and then carrying out polarization treatment on the divided material blocks, or firstly carrying out polarization treatment on the annular piezoelectric single crystal material and then uniformly dividing the annular piezoelectric single crystal material into a plurality of sector-shaped material blocks along the circumferential direction by taking the axis of the annular piezoelectric single crystal material as a center; and selecting a plurality of material blocks with similar performance, and reassembling the material blocks into a ring in a mode that piezoelectric performance signs between the adjacent material blocks are opposite. According to the invention, the piezoelectric single crystal element with high piezoelectric property uniformity can be efficiently obtained, and the defects of nonuniform piezoelectric property distribution, fragility and the like caused by component segregation and a polarization process are effectively avoided.
Description
Technical Field
The invention belongs to the technical field of piezoelectric single crystal element preparation, and particularly relates to a preparation method of a piezoelectric single crystal element.
Background
The piezoelectric material can generate voltage between two end faces when being stressed by pressure, so that the piezoelectric material can realize direct interconversion between mechanical energy and electric energy, is a very important functional material, is widely applied to the fields of aviation, energy, automobile manufacturing, communication, detection, household appliances, computers and the like, is an important component part for forming electronic elements such as a transducer, a filter, a sensor, a driver and the like, and has become one of the main research directions of high and new technologies in the 21 st century.
Binary piezoelectric ceramic lead zirconate titanate (PZT) ceramics have been widely used for more than half a century because of their higher piezoelectric performance and serialized material products. However, with the continuous development of science and technology, a new generation of high performance piezoelectric single crystal-relaxor ferroelectric single crystal is appeared, which mainly comprises lead zincate niobate-lead titanate (PZNT), lead magnesium niobate titanate (PMNT), lead magnesium niobate titanate (PIMNT), and the like.
The piezoelectric single crystal material has excellent piezoelectric performance, such as piezoelectric constant d33More than 1500pC/N, 4-5 times higher than PZT ceramic, 1.7% higher than PZT ceramic, one order of magnitude higher than PZT ceramic, and electromechanical coupling factor k33The piezoelectric ceramic reaches more than 90 percent and is remarkably higher than the electromechanical coupling factor of about 70 percent of PZT ceramic, so the piezoelectric ceramic is considered as one of the most exciting breakthroughs in the piezoelectric field for 50 years, and causes great attention of scholars in the ferroelectric and piezoelectric fields. In addition to this, the relaxor ferroelectric single crystal has exceptionally excellent low-temperature properties. The performance of the conventional PZT ceramic series piezoelectric ceramic is reduced by 75% at a temperature of-240 ℃ because of the increase of hysteresis loss when the temperature is reduced to-40 ℃. However, the piezoelectric performance of the relaxor ferroelectric single crystal at-240 ℃ is still superior to that of the piezoelectric ceramic at 30 ℃.
The excellent performance of the relaxor ferroelectric single crystal enables the relaxor ferroelectric single crystal to be widely applied to the fields of underwater acoustic transducers, medical B-ultrasonic, ultrasonic motors and the like. The ultrasonic motor is manufactured according to the inverse piezoelectric effect of a piezoelectric material, and compared with a common electrode, the ultrasonic motor has the advantages of high torque density, low-voltage input, high-precision positioning, short response time, good displacement repeatability, low consumption, no need of lubrication, no electromagnetic interference and the like. The piezoelectric material is a component for converting electric energy into vibration energy in the ultrasonic motor, and the advantages and disadvantages of the piezoelectric material are related to the mechanical characteristics of the ultrasonic motor.
The polarization process is a key process for obtaining piezoelectric performance of the piezoelectric material, particularly the piezoelectric material partition polarization process, one piezoelectric material is divided into a plurality of areas, and the directions of electric fields applied when adjacent areas are polarized are opposite. The current mature polarization process is mainly developed aiming at the traditional piezoelectric PZT ceramic, such as different area polarization by time or all areas polarization simultaneously. However, due to the characteristics of component segregation and the like of the piezoelectric single crystal, the traditional polarization process is difficult to obtain the zoned polarization piezoelectric element with high piezoelectric uniformity.
Disclosure of Invention
The problems to be solved by the invention are as follows:
as described above, if different regions are subjected to polarization processing for several times as in the conventional piezoelectric PZT ceramics, piezoelectric properties of piezoelectric single crystal materials such as PIMNT, PMNT, PZNT are not uniform due to an inappropriate polarization process, and if all regions are subjected to polarization processing simultaneously, the piezoelectric single crystal materials are brittle.
In addition, due to component segregation of piezoelectric single crystal materials such as PIMNT, PMNT and PZNT in the growth process, the performance distribution of the piezoelectric single crystal materials is uneven, if the piezoelectric single crystal materials are not spliced and are polarized after being directly partitioned, and due to the fact that the performance of the piezoelectric single crystal materials is uneven, the piezoelectric performance of the annular piezoelectric single crystal element is also uneven. Further, if the piezoelectric performance uniformity of each region of the piezoelectric single crystal element is low, the amplitudes of two standing waves excited by the piezoelectric vibrator are not equal. Therefore, the contact surface fluctuates in the axial direction of the motor, the running stability of the ultrasonic motor is influenced, the working efficiency of the ultrasonic motor is reduced, and noise is also generated.
In view of the above problems, an object of the present invention is to provide a method for manufacturing a piezoelectric single crystal element that can effectively avoid the non-uniform piezoelectric property distribution caused by segregation of piezoelectric single crystal components and a polarization process.
The technical means for solving the problems are as follows:
the present invention provides a method for manufacturing a piezoelectric single crystal element, comprising:
firstly, preparing an annular piezoelectric single crystal material and coating a conductive electrode on the surface of the piezoelectric single crystal material;
secondly, the piezoelectric single crystal material is divided and polarized:
firstly, equally dividing the annular piezoelectric single crystal material into a plurality of sector-shaped material blocks along the circumferential direction by taking the axis of the piezoelectric single crystal material as a center, and then carrying out polarization treatment on the divided material blocks, or firstly carrying out polarization treatment on the annular piezoelectric single crystal material, and then equally dividing the piezoelectric single crystal material into a plurality of sector-shaped material blocks along the circumferential direction by taking the axis of the piezoelectric single crystal material as a center;
thirdly, a plurality of material blocks with similar performance are selected and are assembled into a ring again in a mode that piezoelectric performance signs between the adjacent material blocks are opposite.
The preparation method of the piezoelectric single crystal element is mainly used for preparing the piezoelectric single crystal material zoned polarization element. Specifically, a plurality of annular piezoelectric single crystal materials are cut into a plurality of material blocks, the material blocks with similar performance are selected to form a group, and then the annular piezoelectric single crystal elements are assembled. Therefore, the piezoelectric single crystal element with high piezoelectric property uniformity can be efficiently obtained under the condition that the piezoelectric single crystal material has uneven performance, and the defects of uneven piezoelectric property distribution, frangibility and the like caused by component segregation and polarization processes of the piezoelectric single crystal material are effectively avoided, so that the piezoelectric single crystal material can be well applied to piezoelectric devices such as ultrasonic motors and the like.
In the present invention, adjacent material blocks may be bonded to each other by a nonconductive material. This enables the piezoelectric material to be bonded in a ring shape.
In the present invention, the nonconductive substance may be a mixture of an epoxy resin and a curing agent, or a sulphoaluminate cement. Therefore, the piezoelectric material can be well bonded through the material, and acoustic impedance matching is also good.
In the present invention, the piezoelectric single crystal material may be lead zincate niobate-lead titanate (PZNT), lead magnesium niobate titanate (PMNT), or lead magnesium niobate titanate niobate indium niobate (PIMNT). Therefore, the materials have the best industrial prospect in the relaxor ferroelectric piezoelectric single crystal at present, the materials can be subjected to zone polarization, almost all available products can be obtained, and the application range is wide.
In the invention, the diameter of the inner circle of the piezoelectric single crystal material is 0.5 mm-90 mm, the diameter of the outer circle is 2 mm-100 mm, and the thickness is 0.2-50 mm. This enables the size of the ring-shaped piezoelectric material for the driver to be covered.
In the invention, the electric field applied during the polarization treatment is E, and Ec is less than or equal to E and less than or equal to 10Ec, wherein Ec is the coercive field of the polarized crystal material; the temperature during the polarization treatment is T, the room temperature is more than or equal to T and less than or equal to Td, wherein Td is the depolarization temperature of the piezoelectric single crystal material; the time of the polarization treatment is t, and t is more than or equal to 1 s. Therefore, Ec is less than or equal to E and less than or equal to 10Ec is the polarization condition usually selected by the laboratory, which can ensure that the piezoelectric element can be polarized and can not crack the sample because of the high applied electric field. The temperature range used in polarization is covered by Td which is less than or equal to the room temperature, the room temperature sample can be polarized, the higher the temperature is, the easier the electric domain is to be switched, the lower the polarization electric field needs to be applied in polarization, but when the temperature is higher than Td, the piezoelectric performance of the sample is degraded, and the sample can not be polarized at the temperature beyond the temperature. As the polarization process is the diversion process of the electric domain in the sample, the common polarization time in a laboratory is 10-30min to ensure that a single domain has enough time to divert, but theoretically the electric domain diversion time is fast and can be completed within 1 second, so the polarization treatment time is only longer than the time.
The invention has the following effects:
the invention can provide a preparation method of the piezoelectric single crystal element, which can effectively avoid the defects of uneven piezoelectric property distribution, frangibility and the like caused by segregation of piezoelectric single crystal components and a polarization process.
Drawings
FIG. 1 is a schematic structural view of a piezoelectric single-crystal element obtained by the method according to embodiment 1 of the invention;
FIG. 2 is a schematic structural view of a piezoelectric single-crystal element obtained by the method according to embodiment 2 of the invention;
FIG. 3 is a schematic structural view of a piezoelectric single-crystal element obtained by the method according to embodiment 3 of the invention;
fig. 4 is a schematic structural view of a piezoelectric single-crystal element obtained by the method according to embodiment 4 of the present invention.
Detailed Description
The present invention is further described below in conjunction with the following embodiments, which are to be understood as merely illustrative, and not restrictive, of the invention. The same or corresponding reference numerals denote the same components in the respective drawings, and redundant description is omitted.
The preparation method of the piezoelectric single crystal element is mainly suitable for the sectional polarization of piezoelectric single crystal materials, and can provide an effective preparation process for preparing the piezoelectric single crystal element by sectional polarization of a new generation of piezoelectric single crystal materials, namely relaxor ferroelectric single crystal materials. Specifically, at least one piezoelectric single crystal material in a ring shape is prepared, and a conductive electrode is coated on the surface.
Each piezoelectric single crystal material is then divided and polarized. The order of the division and polarization treatment is not limited, and may be changed as needed. For example, the ring-shaped piezoelectric single crystal material may be divided into several pieces of sector-shaped material, and then the divided pieces of material may be subjected to polarization treatment. Specifically, the piezoelectric single crystal material is divided equally in the circumferential direction thereof around the axis of the ring, thereby obtaining a plurality of blocks of piezoelectric single crystal material having a sector-shaped cross section. Alternatively, the piezoelectric single crystal material may be subjected to the above-described polarization treatment and then subjected to the above-described division. The cross section referred to in the present invention is a cross section cut by a plane perpendicular to the axial direction of the annular piezoelectric single crystal material.
And then, after the material blocks are mixed, selecting material blocks with similar performance from the material blocks, and regrouping the material blocks, wherein the number of the piezoelectric single crystal materials prepared by the first English component quantity is consistent, and each group is internally provided with the same number of material blocks. Finally, the material blocks are assembled into a closed ring shape in a mode that piezoelectric performance signs between the adjacent material blocks are opposite, and the material blocks are bonded through the non-conductive substance. Theoretically, the number of piezoelectric single crystal elements produced finally coincides with the number of piezoelectric single crystal materials produced initially. In the invention, the two ends of the ring-shaped piezoelectric single crystal material after polarization treatment have opposite piezoelectric performance signs, and after the ring-shaped piezoelectric single crystal material is divided, the opposite piezoelectric performance signs between the adjacent material blocks can be realized only by inverting the upper end and the lower end of the adjacent material blocks, but the invention is not limited to the method in the example.
In the present invention, preferably, the electric field applied during the polarization treatment is E, Ec ≦ E ≦ 10Ec, where Ec is the coercive field of the polarized crystal material. The temperature during the polarization treatment is T, the room temperature is more than or equal to T and less than or equal to Td, wherein Td is the depolarization temperature of the piezoelectric single crystal material. The time for polarization treatment is t, and t is more than or equal to 1 s.
In the present invention, the piezoelectric single crystal material may be lead zinc niobate-lead titanate (PZNT), lead magnesium niobate titanate (PMNT), lead magnesium niobate titanate (PIMNT), but is not limited thereto, and for example, PZT ceramics may be used. In addition, in the invention, the inner circle diameter of the piezoelectric single crystal material is preferably 0.5 mm-90 mm, the outer circle diameter is preferably 2 mm-100 mm, and the thickness is preferably 0.2-50 mm. Further, the non-conductive substance used for bonding the block of piezoelectric single crystal material may be a mixture of an epoxy resin and a curing agent, or a sulphoaluminate cement, but is not limited thereto.
According to the preparation method of the piezoelectric single crystal element, the piezoelectric single crystal element with high piezoelectric property uniformity can be efficiently obtained under the condition that the piezoelectric single crystal material has uneven performance, the defects of uneven piezoelectric property distribution, fragility and the like caused by component condensation and polarization processes of the piezoelectric single crystal material are effectively avoided, and therefore the piezoelectric single crystal material can be well applied to piezoelectric devices such as ultrasonic motors.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
(example 1)
Fig. 1 is a schematic structural view of a piezoelectric single-crystal element obtained by the method according to embodiment 1 of the present invention. As shown in fig. 1, the PIMNT crystal was processed into a ring shape in a number of 5, the thickness of the ring-shaped PIMNT crystal was 2mm, the inner diameter was 20mm, the outer diameter was 30mm, and the upper and lower surfaces were coated with conductive electrodes. Firstly, the material is polarized, wherein the electric field applied during the polarization treatment is 1.5KV, the polarization temperature is 50 ℃, and the polarization time is 30 minutes. Each annular PIMNT crystal is then cut into 10 equal blocks of material, for a total of 50 for 5 PIMNT crystals. The blocks are detected and divided into 5 groups according to the level of the piezoelectric performance, and the piezoelectric performance of each group is similar. Finally, the mixture of epoxy resin and room temperature curing agent is utilized to re-bond the 10 material blocks in each group into a closed annular piezoelectric single crystal element, and the piezoelectric performance signs between the adjacent material blocks are ensured to be opposite during assembly.
The following table shows the piezoelectric properties of three samples in the piezoelectric single-crystal element obtained by the method of example 1 according to the present invention;
therefore, the piezoelectric single crystal material is not cracked and has good performance after being subjected to zone polarization.
(example 2)
Fig. 2 is a schematic structural view of a piezoelectric single-crystal element obtained by the method according to embodiment 2 of the present invention. As shown in fig. 2, the PMNT crystal was processed into a ring shape, the number of which was 10, the thickness of the ring-shaped PMNT crystal was 3mm, the inner diameter was 16mm, the outer diameter was 32mm, and the upper and lower surfaces thereof were coated with conductive electrodes. First, each ring-shaped PMNT crystal was cut into 8 equal blocks of material, with 10 PMNT crystals totaling 80 blocks of material. Then, 80 blocks of material were subjected to polarization treatment with an electric field of 1.8KV, a polarization temperature of room temperature, and a polarization time of 10 minutes. The material blocks are detected and divided into 10 groups according to the level of the piezoelectric performance, and the piezoelectric performance of each group is similar. Finally, 8 material blocks in each group are bonded again into a closed annular piezoelectric single crystal element by utilizing sulphoaluminate cement, and the piezoelectric performance signs between the adjacent material blocks are ensured to be opposite during assembly.
The following table shows the piezoelectric properties of three samples in the piezoelectric single-crystal element obtained by the method of example 2 according to the present invention;
therefore, the piezoelectric single crystal material is not cracked and has good performance after being subjected to zone polarization.
(example 3)
Fig. 3 is a schematic structural view of a piezoelectric single-crystal element obtained by the method according to embodiment 3 of the present invention. As shown in fig. 3, the PZNT crystal was processed into a ring shape in 20 pieces, the thickness of the ring-shaped PZNT crystal was 1mm, the inner diameter was 8mm, the outer diameter was 14mm, and the upper and lower surfaces thereof were coated with conductive electrodes. First, the substrate was subjected to polarization treatment in which an electric field of 1KV was applied, a polarization temperature of 125 ℃ and a polarization time of 3 minutes were applied. Each annular PZNT crystal was then cut into 6 equal blocks of material, with a total of 120 blocks of 20 PZNT crystals. The blocks are detected and divided into 20 groups according to the level of the piezoelectric performance, and the piezoelectric performance of each group is similar. Finally, the mixture of epoxy resin and room temperature curing agent is utilized to re-bond the 6 material blocks in each group into a closed annular piezoelectric single crystal element, and the piezoelectric performance signs between the adjacent material blocks are ensured to be opposite during assembly.
The following table shows the piezoelectric properties of three samples in the piezoelectric single-crystal element obtained by the method of example 3 according to the present invention;
therefore, the piezoelectric single crystal material is not cracked and has good performance after being subjected to zone polarization.
(example 4)
Fig. 4 is a schematic structural view of a piezoelectric single-crystal element obtained by the method according to embodiment 4 of the present invention. As shown in fig. 4, the PIMNT crystal was processed into a ring shape in a number of 100, the thickness of the ring-shaped PIMNT crystal was 4mm, the inner diameter was 10mm, the outer diameter was 25mm, and the upper and lower surfaces thereof were coated with conductive electrodes. First, the resultant was subjected to a polarization treatment in which an electric field of 5KV was applied, a polarization temperature was 135 ℃ and a polarization time was 45 minutes. Each annular PIMNT crystal is then cut into 12 equal blocks of material, for a total of 1200 blocks of PIMNT crystals for 100. The material blocks are detected and divided into 100 groups according to the level of the piezoelectric performance, and the piezoelectric performance of each group is similar. 12 material blocks in each group are bonded into a closed annular piezoelectric single crystal element by utilizing sulphoaluminate cement, and the piezoelectric performance signs between the adjacent material blocks are ensured to be opposite during assembly.
The following table shows the piezoelectric properties of three samples in the piezoelectric single-crystal element obtained by the method of example 4 according to the present invention;
therefore, the piezoelectric single crystal material is not cracked and has good performance after being subjected to zone polarization.
The invention develops a new preparation method of a piezoelectric single crystal element, which is mainly used for preparing a piezoelectric single crystal material partitioned polarization element and can provide an effective preparation process for preparing a new generation of piezoelectric single crystal material, namely a relaxor ferroelectric single crystal material partitioned polarization element. The method can successfully and efficiently prepare the piezoelectric single crystal element with high piezoelectric property uniformity, and effectively avoid the defects of nonuniform piezoelectric property distribution, fragility and the like caused by component condensation of piezoelectric single crystal materials and a polarization process, so that the piezoelectric single crystal element can be well applied to piezoelectric devices such as an ultrasonic motor and the like, and the market compatibility is improved.
The above embodiments are intended to illustrate and not to limit the scope of the invention, which is defined by the claims, but rather by the claims, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims (6)
1. A method for manufacturing a piezoelectric single crystal element, comprising:
firstly, preparing an annular piezoelectric single crystal material and coating a conductive electrode on the surface of the piezoelectric single crystal material;
secondly, the piezoelectric single crystal material is divided and polarized:
firstly, equally dividing the annular piezoelectric single crystal material into a plurality of sector-shaped material blocks along the circumferential direction by taking the axis of the piezoelectric single crystal material as a center, and then carrying out polarization treatment on the divided material blocks, or firstly carrying out polarization treatment on the annular piezoelectric single crystal material, and then equally dividing the piezoelectric single crystal material into a plurality of sector-shaped material blocks along the circumferential direction by taking the axis of the piezoelectric single crystal material as a center;
thirdly, a plurality of material blocks with similar performance are selected and are assembled into a ring again in a mode that piezoelectric performance signs between the adjacent material blocks are opposite.
2. A method of manufacturing a piezoelectric single crystal element according to claim 1, wherein adjacent material blocks are bonded to each other by a non-conductive substance.
3. A method of manufacturing a piezoelectric single crystal element according to claim 2, wherein the non-conductive substance is a mixture of an epoxy resin and a curing agent, or a sulphoaluminate cement.
4. The method of producing a piezoelectric single crystal element according to claim 1, wherein the piezoelectric single crystal material is lead zincate niobate-lead titanate (PZNT), lead magnesium niobate titanate (PMNT), or lead magnesium niobate titanate (PIMNT).
5. A method for manufacturing a piezoelectric single crystal element according to claim 1, wherein the piezoelectric single crystal material has an inner circle diameter of 0.5mm to 90mm, an outer circle diameter of 2mm to 100mm, and a thickness of 0.2 mm to 50 mm.
6. The method of claim 1, wherein the electric field applied during the poling process is E, Ec is less than or equal to E and less than or equal to 10Ec, wherein Ec is the coercive field of the poled crystal material;
the temperature during the polarization treatment is T, the room temperature is more than or equal to T and less than or equal to Td, wherein Td is the depolarization temperature of the piezoelectric single crystal material;
the time of the polarization treatment is t, and t is more than or equal to 1 s.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112260576A (en) * | 2020-10-30 | 2021-01-22 | 西安科技大学 | Single crystal splicing method for annular ultrasonic motor |
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Application publication date: 20200728 |