CN114149258A - Piezoelectric ceramic with laminated structure and preparation method and application thereof - Google Patents

Piezoelectric ceramic with laminated structure and preparation method and application thereof Download PDF

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CN114149258A
CN114149258A CN202111638970.0A CN202111638970A CN114149258A CN 114149258 A CN114149258 A CN 114149258A CN 202111638970 A CN202111638970 A CN 202111638970A CN 114149258 A CN114149258 A CN 114149258A
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piezoelectric ceramic
laminated structure
ceramic powder
powder
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CN114149258B (en
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王妍
陈川
张熙民
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Super High Voltage Co Of State Grid Shandong Electric Power Co
Global Energy Interconnection Research Institute
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Super High Voltage Co Of State Grid Shandong Electric Power Co
Global Energy Interconnection Research Institute
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Abstract

The invention discloses a piezoelectric ceramic with a laminated structure and a preparation method and application thereof. The preparation method of the piezoelectric ceramic with the laminated structure comprises the following steps: obtaining raw material powder: obtaining at least two systems of piezoelectric ceramic powder materials with different Curie temperature points, taking corresponding components of multiphase coexisting points of respective systems as cores, and respectively selecting the cores and components with the floating rate of the two sides within 15% as the piezoelectric ceramic powder materials; and (3) preparing a finished product: after the piezoelectric ceramic powder is overlapped layer by layer to form a semi-finished product with a laminated structure, sintering, cleaning, cutting and splashingAnd (5) injecting to obtain a finished product. The electrostriction of the piezoelectric ceramic with the laminated structure prepared by the invention almost expresses higher electrostriction in a single component at different temperatures, namely the piezoelectric ceramic with the laminated structure has the peak value in the temperature range and BTS0.105Piezoelectric ceramic and BTH0.11The peak value of the piezoelectric ceramic is equivalent to or even higher, and the piezoelectric ceramic has comprehensive effects.

Description

Piezoelectric ceramic with laminated structure and preparation method and application thereof
Technical Field
The invention relates to the technical field of piezoelectric ceramics, in particular to piezoelectric ceramics with a laminated structure and a preparation method and application thereof.
Background
Piezoelectric ceramics are often used as position regulators in optical and microelectronic systems, and are often required to generate large driving force and mechanical strain under the excitation action of an external electric field, and the performance can be accurately and intuitively evaluated by testing the magnitude of the electrical strain of the material.
The electrostriction of piezoelectric ceramics derives from three contributions: the first is an intrinsic nonlinear strain mechanism, which originates from the electrostrictive effect of the material, caused by induced polarization, and is present in almost all dielectrics; the second is the inverse piezoelectric effect existing only in the non-centrosymmetric crystal material, and is an intrinsic linear strain mechanism; the third is the source of extrinsic strain due to non-180 ° ferroelectric domain inversion.
For a ferroelectric piezoelectric material, corresponding strain response is carried out on the change of polarization strength corresponding to a ferroelectric hysteresis loop, when the intensity of an externally applied electric field is small, only induced polarization is generated in the piezoelectric material, and only electrostrictive effect with small numerical value is contained in electrostrictive strain; however, when the external field strength exceeds the polarization field strength, the randomly distributed ferroelectric domains in the ferroelectric piezoelectric material gradually orient uniformly along the electric field direction to form a single domain structure, so that a large inverse piezoelectric effect is generated, and the strain response linearly increases along with the increase of the electric field and reaches the maximum at the maximum field strength.
In recent years, researchers have found that there is always an abnormal increase in various physical properties at the ferroelectric-ferroelectric phase boundary of ferroelectric piezoelectric materials, such as lead-based (0.2Pb (Mg) (for example)1/3Nb2/3)O3-xPbZrO3-(0.8-x)PbTiO3、Pb1-3/2xLax(Zr1- yTiy)O3) And lead-free systems (BaTiO)3Radical, (Bi)0.5Na0.5)TiO3Radical, (K, Na) NbO3Basal) temperature-component phase diagram, the dielectric constant, piezoelectric coefficient and electrostrictive coefficient all show maximum values at the Morphotropic Phase Boundary (MPB). The scholars believe that the enhanced electrostrictive strain at the phase boundary results from phase instability at the phase boundary, i.e., the tendency for the different phases to switch under the action of an applied electric field.
In practice, piezoelectric ceramics should not only take into account a high electrical strain coefficient as a driver, but also have reliable temperature stability. The existing method for improving the temperature stability of the piezoelectric ceramic electrostriction mainly focuses on element doping, and the method has limited improvement degree of the temperature stability and certain randomness.
Disclosure of Invention
Therefore, the technical problem to be solved by the present invention is to overcome the defects of limited improvement degree and certain randomness existing in the prior art for improving the piezoelectric ceramic electrostrictive temperature stability by element doping, so as to provide a method for preparing a piezoelectric ceramic with a laminated structure, wherein the temperature stability is obviously improved while high electrostrictive strain is maintained.
A method for preparing a piezoelectric ceramic having a laminated structure, comprising:
obtaining raw material powder: obtaining at least two systems of piezoelectric ceramic powder materials with different Curie temperature points, taking corresponding components of multiphase coexisting points of respective systems as cores, and respectively selecting the cores and components with the floating rate of the two sides within 15% as the piezoelectric ceramic powder materials;
and (3) preparing a finished product: the piezoelectric ceramic powder is superposed layer by layer to form a semi-finished product with a laminated structure, and then the semi-finished product is sintered, cleaned, cut and sputtered to form a finished product.
The preparation process of the semi-finished product comprises the following steps:
pre-pressing: pressing different piezoelectric ceramic powder materials layer by layer under the pressure of 2-3MPa for more than 0.5min to form a laminated sample;
pressing: and putting the laminated sample into a sealed bag, vacuumizing, and pressing under the condition of cold isostatic pressure of 200MPa to prepare a semi-finished product.
In the pre-pressing step, the pressing time of each layer of piezoelectric ceramic powder before the last time is 0.5-3min, preferably 1 min; the pressing time of the last layer of piezoelectric ceramic powder is more than 5min, preferably 5 min.
In the pressing step, the pressing time is 3min or more, preferably 3 min.
The piezoelectric ceramic powders of the two systems are respectively doped with Sn4+BaTiO of (5)3Base piezoelectric ceramic powder and doped Hf4+BaTiO of (5)3A base piezoelectric ceramic powder.
Doped Sn4+BaTiO of (5)3The core corresponding component of the base piezoelectric ceramic powder is BTSxAnd x is BaSnO3The amount of the substances in the whole, wherein x is 0.105; doping of Hf4+BaTiO of (5)3The core corresponding component of the base piezoelectric ceramic powder is BTHyAnd y denotes BaHfO3The percentage of the total mass, y, is 0.11.
The preparation process of the piezoelectric ceramic powder comprises the following steps: obtaining raw materials according to corresponding components of the piezoelectric ceramic powder, performing wet ball milling on the raw materials to uniformly mix raw material powder, and then drying and calcining the raw material powder; and grinding the calcined sample into powder, performing secondary ball milling on the powder, drying and grinding the powder again to prepare the piezoelectric ceramic powder.
The grinding beads of the wet ball milling are agate balls, and the grinding beads of the secondary ball milling are alumina balls;
the rotation speed of the wet ball milling and the secondary ball milling is 600r/min, the time of the wet ball milling is 4 hours, and the time of the secondary ball milling is 8 hours;
the liquid added during the wet ball milling is absolute ethyl alcohol;
the calcining temperature is 1350 ℃ and the calcining time is 3 h.
In the step of preparing the finished product, the sintering temperature is 1450 ℃, and the sintering time is 3 hours;
cutting the rectangular body along the direction of component change during the cutting;
the sputtering process comprises the following steps: and (3) carrying out gold spraying treatment on two parallel planes with variable components by using an ion sputtering instrument, wherein each plane is sputtered for 2-3 times.
The piezoelectric ceramic with a laminated structure prepared by the preparation method of the piezoelectric ceramic with a laminated structure is provided.
The preparation method of the piezoelectric ceramic with the laminated structure is applied to improving the temperature stability of the piezoelectric ceramic in electrostriction.
The technical scheme of the invention has the following advantages:
1. the invention provides a preparation method of piezoelectric ceramic with a laminated structure, which adopts at least two systems of piezoelectric ceramic powder materials with different Curie temperature points, and constructs the laminated structure near the corresponding components of the multiphase coexistence point (three critical points) of the piezoelectric ceramic powder materials of each system, so that the temperature stability of the piezoelectric ceramic material is improved while high electrostrictive strain is kept.
2. In the preparation method of the piezoelectric ceramic with the laminated structure, a mode of prepressing layer by layer under a low-pressure condition and finally pressing and preparing under a vacuum high-pressure condition is adopted; the method has no strict requirements on components, and even if the component difference is large, the phenomenon of layering can not occur, so that the preparation method has more freedom; in addition, the finished product prepared by the method is more compact and has better performance; the temperature stability of the electrostrictive strain performance of materials of different systems is obviously adjusted, and more importantly, the performance peak value of the new material is equivalent to the level of the single material after adjustment.
Compared with the traditional method for improving the electrostrictive strain stability of the piezoelectric ceramic, the method provided by the invention has the advantages of simplicity and convenience in operation and easiness in control.
3. The electrostriction of the piezoelectric ceramic with the laminated structure prepared by the invention almost expresses higher electrostriction in a single component at different temperatures, and the piezoelectric ceramic has comprehensive effect, so that the electrostriction in a certain temperature range can be purposefully improved by adjusting the components of each layer when the laminated material is designed, and the result predictability is achieved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is an electrostrictive strain of the finished product prepared in example 1 of the present invention at a temperature ranging from 25 to 75 ℃;
FIG. 2 is a BTS of the present invention0.105An electric strain diagram of the piezoelectric ceramic in a temperature range of 25-75 ℃;
FIG. 3 shows BTH of the present invention0.11An electric strain diagram of the piezoelectric ceramic in a temperature range of 25-75 ℃;
FIG. 4 shows BTS, a finished product obtained in example 1 of the present invention0.105Piezoelectric ceramic and BTH0.11The peak change diagram of the electric strain of the piezoelectric ceramics at the temperature of 25-75 ℃.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
Considering the optimization of the electrostriction and the temperature stability of the piezoelectric ceramic in the room temperature and the normal heating temperature range of the device, which is around 25-75 ℃, a barium titanate system doped with Sn4+ and Hf4+ is selected, and the temperature of the multiphase coexisting point of the barium titanate system and the multiphase coexisting point of the barium titanate system is 37 ℃ and 70 ℃, so that the electrostriction and the temperature stability of the piezoelectric ceramic are improved by combining a plurality of components around the multiphase coexisting point.
(1) For doping with Sn4+Of barium titanate system, i.e. Ba (Ti)1-xSnx)O3(BTSx) And x is BaSnO3The percentage of the total substance is shown by the research that the corresponding component of the multiphase coexisting point of the system is BTS0.105. For doping Hf4+Of barium titanate system, i.e. Ba (Ti)1-yHfy)O3(BTHy) And y denotes BaHfO3The percentage of the total substance is shown by the research that the corresponding component of the multiphase coexisting point of the system is BTS0.11。
(2) BTS centered on a component with x equal to 0.1050.105Selecting 1 component point on both sides, sequentially BTS according to Curie temperature from low to high (doping percentage from large to small)0.12、BTS0.105And BTS0.09(ii) a BTH centered on the component y of 0.110.11Selecting 1 component point on both sides, sequentially BTH from low Curie temperature to high Curie temperature (doping percentage from large to small)0.13、BTH0.11And BTH0.09(ii) a Based on these six components, a piezoelectric ceramic having a laminated structure of six layers components, whose Curie temperatures are 23 ℃, 37 ℃, 47 ℃, 58 ℃, 70 ℃ and 84 ℃ respectively, is constituted.
(3) Weighing the doped Sn according to the theoretical calculation result of the component percentage4+Ions and Hf4+The raw materials required for 25g of each component of the ionic barium titanate piezoelectric ceramic system are shown in tables 1 and 2.
TABLE 1 BTSxThe mass ratio of each raw material
Figure BDA0003443446870000071
TABLE 2 BTHyThe mass ratio of each raw material
Figure BDA0003443446870000072
(4) Before ball milling raw materials, pure water is firstly filled into a ball milling tank for ball milling until liquid is clear and no impurities exist, then alcohol is filled into the ball milling tank for ball milling for half an hour, and the ball milling tank is numbered in advance. The combined raw materials for each component were then placed into the corresponding numbered tanks and the sample was slightly immersed by pouring about 1/3 volumes of absolute ethanol. The rotation speed of the primary ball milling is 600r/min, and the time is 4 hours (the primary ball milling can be pre-rotated for 5min to check whether the installation is tight or not). The purpose of the primary ball milling is to uniformly mix the weighed raw material powder.
(5) Pouring the ball-milled sample into a culture dish, covering filter paper on the culture dish, and putting the culture dish into an oven to be dried for about 5 hours until the surface of the alcohol volatilization sample is cracked. After drying, it was poured into a mortar and ground to a finer powder and compacted into numbered small crucibles. The zirconium plate is firstly padded in a box-type furnace, four crucibles are placed on the zirconium plate, and then the zirconium plate is covered for calcination. The temperature of calcination was 1350 ℃ and the time was 3 hours.
(6) And crushing the calcined ceramic sample, grinding the crushed ceramic sample into fine powder again, carrying out secondary ball milling, and replacing the agate balls with alumina ball milling beads with the same size. The rotation speed of the secondary ball milling is 600r/min, and the time is 8 hours, so that the particle size of the powder is more uniform.
(7) And drying the sample subjected to the secondary ball milling for 5 hours, and pouring the dried sample into a mortar to be ground into powder.
(8) Weigh 0.3g of BTS0.12Pouring into 10mm mold, pre-pressing at 3MPa for 1min to make sample surface flat, sequentially adding BTS0.105、BTS0.09、BTH0.13、BTH0.11And BTH0.09The sample powders, 0.3g per layer, were pre-compacted in the same way as the pre-compaction. After all the components are pre-pressed, the last time is kept for 5 minutes. And putting the pre-pressed sample into a latex bag, vacuumizing, putting the latex bag into a cold isostatic press, and pressing the latex bag into a compact laminated structure ceramic sample at the pressure of 200MPa for 3 min.
(9) And sintering the pressed and molded sample by a box furnace in a buried burning mode. Sintering is the binding of powders into a dense mass by mechanisms such as creep, diffusion, localized melting, and the like. The sintering temperature is 1450 ℃, and the sintering time is 3 hours. The sintering temperature is generally higher than the calcination temperature for dense forming.
(10) The powder buried and burned in the surface of the laminated ceramic sample was polished with fine sandpaper, and the ceramic was cut into a rectangular block in the direction of change of composition using a precision line cutter according to the advance mark.
(11) And (3) carrying out metal spraying treatment on two parallel planes with component change by using an ion sputtering instrument, and sputtering each plane for 3 times to obtain the piezoelectric ceramics with the laminated structures in parallel.
Example 2
The difference between this example and example 1 is that the step (8) in example 1 is different, specifically, in this example, piezoelectric ceramic powder is spread and leveled layer by layer, and then pressed for 3min under the condition of cold isostatic pressure of 20MPa to prepare a semi-finished product, and the other steps are the same as example 1.
Example 3
The present example differs from example 1 in that, unlike step (8) in example 1 described above, specifically, in this example, 0.3g of BTS was weighed0.12Pouring into 10mm mold, pre-pressing for 0.5min under 2MPa to make sample surface flat, and sequentially adding BTS 0.3g each time0.105、BTS0.09、BTH0.13、BTH0.11And BTH0.09And (4) prepressing the sample powder in the same prepressing mode. After all the components are pre-pressed, the last time is kept for 7 min. And putting the pre-pressed sample into a latex bag, vacuumizing, putting the latex bag into a cold isostatic press, and pressing the latex bag into a compact laminated structure ceramic sample at the pressure of 200MPa for 5 min.
Test examples
Piezoelectric ceramic having a laminated structure prepared in example 1, and BTS0.105Piezoelectric ceramic and BTH0.11The piezoelectric ceramics carry out the electrostrictive strain detection within the temperature range of 25-75 ℃, and the specific detection process is as follows:
respectively measuring by a TF Analyzer 2000E ferroelectric AnalyzerThe variation of the electrical strain of 2kV/mm of different samples at 25 deg.C, 35 deg.C, 45 deg.C, 55 deg.C, 65 deg.C and 75 deg.C is tested, as shown in FIGS. 1-3. Wherein FIG. 1 is a graph showing the results of the piezoelectric ceramic having a laminated structure prepared in example 1, and FIG. 2 is BTS0.105FIG. 3 is a BTH graph showing the results of piezoelectric ceramics0.11And (4) a result graph of the piezoelectric ceramics. As can be seen by comparing fig. 1 and fig. 2-3: in the temperature range, the peak value of the electrostriction of the piezoelectric ceramic prepared by the invention is only slightly reduced along with the temperature increase, and BTS0.105The peak value of the piezoelectric ceramic is obviously reduced along with the temperature increase, and BTH0.11The peak value of the piezoelectric ceramic increases and then decreases with increasing temperature.
In order to compare the electrical strain and its temperature stability of the laminate and the three critical materials that make up it more clearly, we show the peak values of the electrical strain at different temperatures of the three materials simultaneously in fig. 2, which can be visualized by fig. 2: the laminated material not only maintains higher electrostriction, but also has excellent temperature stability. It is thus possible to verify: the laminated structure effectively realizes that the temperature stability of the electrical strain is improved on the basis of keeping higher electrical strain of the system ceramic.
In addition, the electrical strain of the piezoelectric ceramic having a laminated structure almost expresses a higher electrical strain in a single component at different temperatures, that is, the peak values of the piezoelectric ceramic having a laminated structure in the temperature range of the present invention are equal to those of BTS0.105Piezoelectric ceramic and BTH0.11The peak value of the piezoelectric ceramic is equivalent to or even higher, and the piezoelectric ceramic has comprehensive effects.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (10)

1. A method for producing a piezoelectric ceramic having a laminated structure, comprising:
obtaining raw material powder: obtaining at least two systems of piezoelectric ceramic powder materials with different Curie temperature points, taking corresponding components of multiphase coexisting points of respective systems as cores, and respectively selecting the cores and components with the floating rate of the two sides within 15% as the piezoelectric ceramic powder materials;
and (3) preparing a finished product: the piezoelectric ceramic powder is superposed layer by layer to form a semi-finished product with a laminated structure, and then the semi-finished product is sintered, cleaned, cut and sputtered to form a finished product.
2. The method according to claim 1, wherein the process of preparing the semi-finished product comprises:
pre-pressing: different piezoelectric ceramic powder materials are subjected to layer-by-layer treatment under the pressure of 2-3MPa for more than 0.5min to form a laminated sample;
pressing: and putting the laminated sample into a sealed bag, vacuumizing, and pressing under the condition of cold isostatic pressure of 200MPa to prepare a semi-finished product.
3. The method according to claim 2, wherein in the pre-pressing step, the pressing time of each layer of piezoelectric ceramic powder before the penultimate time is 0.5-3min, preferably 1 min; the pressing time of the last layer of piezoelectric ceramic powder is more than 5min, preferably 5 min;
in the pressing step, the pressing time is 3min or more, preferably 3 min.
4. The method according to any one of claims 1 to 3, wherein the piezoelectric ceramic powders of the two systems are each doped with Sn4+BaTiO of (5)3Base piezoelectric ceramic powder and doped Hf4+BaTiO of (5)3A base piezoelectric ceramic powder.
5. The method according to claim 4, wherein Sn is doped4+BaTiO of (5)3The core corresponding component of the base piezoelectric ceramic powder is BTSxAnd x is BaSnO3The amount of the substances in the whole, wherein x is 0.105; doping of Hf4+BaTiO of (5)3The core corresponding component of the base piezoelectric ceramic powder is BTHyAnd y denotes BaHfO3The percentage of the total mass, y, is 0.11.
6. The method according to claim 5, wherein the piezoelectric ceramic powder is prepared by: obtaining raw materials according to corresponding components of the piezoelectric ceramic powder, performing wet ball milling on the raw materials to uniformly mix raw material powder, and then drying and calcining the raw material powder; and grinding the calcined sample into powder, performing secondary ball milling on the powder, drying and grinding the powder again to prepare the piezoelectric ceramic powder.
7. The preparation method according to claim 6, wherein the wet ball-milled milling beads are agate balls, and the secondary ball-milled milling beads are alumina balls;
the rotation speed of the wet ball milling and the secondary ball milling is 600r/min, the time of the wet ball milling is 4 hours, and the time of the secondary ball milling is 8 hours;
the liquid added during the wet ball milling is absolute ethyl alcohol;
the calcining temperature is 1350 ℃ and the calcining time is 3 h.
8. The method according to any one of claims 1 to 7, wherein in the step of preparing the finished product, the sintering temperature is 1450 ℃, and the sintering time is 3 hours;
cutting the rectangular body along the direction of component change during the cutting;
the sputtering process comprises the following steps: and (3) carrying out gold spraying treatment on two parallel planes with variable components by using an ion sputtering instrument, wherein each plane is sputtered for 2-3 times.
9. A piezoelectric ceramic having a laminated structure produced by the method for producing a piezoelectric ceramic having a laminated structure according to any one of claims 1 to 8.
10. Use of the method for preparing a piezoelectric ceramic having a laminated structure according to any one of claims 1 to 9 for improving the temperature stability of electrostrictive strain of a piezoelectric ceramic.
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