CN116082038A - Preparation method of novel ferroelectric ceramic - Google Patents
Preparation method of novel ferroelectric ceramic Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims description 6
- 238000004321 preservation Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052709 silver Inorganic materials 0.000 claims abstract description 11
- 239000004332 silver Substances 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- 238000005498 polishing Methods 0.000 claims abstract description 3
- 239000011812 mixed powder Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 6
- 239000011363 dried mixture Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000003746 solid phase reaction Methods 0.000 abstract 1
- 230000010287 polarization Effects 0.000 description 26
- 230000005684 electric field Effects 0.000 description 25
- 230000007547 defect Effects 0.000 description 20
- 230000002269 spontaneous effect Effects 0.000 description 19
- 230000000694 effects Effects 0.000 description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 230000002950 deficient Effects 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 238000005057 refrigeration Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 2
- 238000001595 flow curve Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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Abstract
The present disclosure discloses a method for preparing a novel ferroelectric ceramic, comprising the steps of: according to the stoichiometry Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3 Pb was weighed separately 3 O 4 、TiO 2 、ZrO 2 And MnO raw material, and sintering into ferroelectric ceramic according to the related steps of a solid phase reaction method; polishing the ferroelectric ceramic, coating silver paste on the upper surface and the lower surface, preserving heat, and naturally cooling to room temperature; and (5) continuing heat preservation treatment on the cooled ferroelectric ceramic.
Description
Technical Field
The present disclosure belongs to the field of solid refrigerating material, and is especially the preparation process of ferroelectric ceramic.
Background
The spontaneous polarization of the ferroelectric ceramic is switched between ordered arrangement and unordered arrangement in the process of applying and removing an electric field, and an exothermic effect and an endothermic effect are generated on the external environment, and the phenomenon is called as an electric card effect and can be used for refrigeration. The refrigeration technology based on the electric card effect has the characteristics of high energy conversion efficiency, no noise, environmental friendliness, integration, easy operation and the like, and becomes a powerful candidate of the next generation refrigeration technology. In general, in an initial state, the ferroelectric ceramic has spontaneous polarization completely in a disordered arrangement state, and the residual polarization is zero. When an external electric field acts for the first time, spontaneous polarization of the ferroelectric ceramic is reversed from a completely disordered state to an ordered state, and large entropy change and large temperature change of the ferroelectric ceramic are generated. However, after the electric field is removed, the spontaneous polarization of the ferroelectric ceramic can only be partially restored to a disordered arrangement state, the entropy change generated at the moment is small, and the temperature change generated by the ferroelectric ceramic is only 0.1-0.3 ℃.
Recent researches find that by doping with proper amount of aliovalent elements, defect dipoles can be introduced into ferroelectric ceramics, and the distribution of the defect dipoles has the same structure as ferroelectric domains after heat preservation. The existence of the defect dipole can provide a restoring force, so that spontaneous polarization after an electric field is removed can be completely restored to a disordered arrangement state, great entropy change is generated, and the corresponding ferroelectric ceramic can also generate great temperature change.
Disclosure of Invention
Aiming at the defects in the prior art, the purpose of the present disclosure is to provide a preparation method of novel ferroelectric ceramic, wherein the defect dipole is formed between the prior ferroelectric ceramic and the oxygen vacancy by doping different valence elements in the prior ferroelectric ceramic, so as to enhance the electric clamping effect of the ferroelectric ceramic.
In order to achieve the above object, the present disclosure provides the following technical solutions:
a preparation method of novel ferroelectric ceramics comprises the following steps:
s1: according to the stoichiometry Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Pb was weighed separately 3 O 4 、TiO 2 、ZrO 2 Mixing with MnO raw materials to obtain a mixture;
s2: ball milling and drying the mixture;
s3: grinding and sieving the dried mixture to obtain mixed powder;
s4: presintering the mixed powder, preserving heat and cooling to room temperature;
s5: grinding and drying the mixed powder cooled to room temperature;
s6: secondary grinding the dried mixed powder, adding PVA with the mass fraction of 8%, uniformly mixing, and sieving to obtain powder with the particle size of 0.15-0.28 mm;
s7: maintaining the pressure of the sieved powder to obtain Pb ((Zr) with the stoichiometric amount 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Is a blank of a blank;
s8: stoichiometric Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Cooling to room temperature after sintering the blank to obtain the stoichiometric Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Ferroelectric ceramics of (a);
s9: stoichiometric Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Polishing the surface of the ferroelectric ceramic, coating silver paste, preserving heat and cooling to room temperature;
s10: the stoichiometric amount of the silver paste which was cooled to room temperature was Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Is used for heat preservation of ferroelectric ceramics.
Preferably, in step S2, the mixture is ball milled for 4-6 hours.
Preferably, in the step S2, the mixture is dried at the temperature of 90-100 ℃ after ball milling.
Preferably, in step S4, the powder mixture is pre-sintered at 1250-1300 ℃.
Preferably, in step S7, the sieved powder is maintained at a pressure of 30MPa for 90-100 seconds.
Preferably, in step S8, the sintering temperature of the green part is 950-1000 ℃.
Preferably, in step S8, the green part is sintered for 4-6 hours.
Preferably, in step S10, the ferroelectric ceramic cooled to room temperature and coated with silver paste is heat-preserved at 430-450 ℃.
Compared with the prior art, the beneficial effects that this disclosure brought are:
the present disclosure is directed to Pb (Zr, ti) O 3 The ferroelectric ceramic is doped with aliovalent element Mn and oxygen vacancy delta, after heat preservation treatment, a defect dipole is formed between the aliovalent element Mn and oxygen vacancy delta, and the distribution of the defect dipole is equal to Pb (Zr, ti) O 3 The ferroelectric ceramics have the same domain structure and can provide a restoring force, so that ferroelectric polarization reversed by an applied electric field can be restored to an initial state, thereby realizing an enhanced electric card effect. The temperature change in ferroelectric ceramics incorporating defective dipoles can generally be greatly enhanced compared to homosystem ferroelectric ceramics not incorporating defective dipoles.
Drawings
FIG. 1 is a flow chart of a method of preparing a novel ferroelectric ceramic according to one embodiment of the present disclosure;
FIG. 2 (a) is a schematic diagram showing an initial state of spontaneous polarization of ferroelectric in the absence of a defective dipole;
FIG. 2 (b) is a schematic diagram showing the arrangement state of spontaneous polarization of ferroelectric under the action of an applied electric field in the absence of a defective dipole;
FIG. 2 (c) is a schematic diagram showing the arrangement state of spontaneous ferroelectric polarization without the presence of a defective dipole;
fig. 2 (d) is a distribution state of spontaneous polarization of the defect dipole and the ferroelectric in the case of introducing the defect dipole and performing a thermal insulation process treatment;
FIG. 2 (e) shows the distribution of the spontaneous polarizations of the defect dipole and the ferroelectric under the action of an applied electric field in the case of introducing the defect dipole;
FIG. 2 (f) shows the distribution of the spontaneous polarizations of the defect dipoles and the ferroelectric under the action of the applied electric field, in the case of introducing the defect dipoles;
FIG. 3 (a) shows the hysteresis loop of a ferroelectric ceramic without heat preservation;
FIG. 3 (b) shows the hysteresis loop of the heat-insulated ferroelectric ceramic;
FIG. 4 (a) is a schematic diagram showing the electrical card effect of the heat-insulated ferroelectric ceramic;
FIG. 4 (b) is a schematic illustration of the electrical card effect of a ferroelectric ceramic without heat preservation.
Detailed Description
Specific embodiments of the present disclosure will be described in detail below with reference to fig. 1 to 4 (b). While specific embodiments of the disclosure are shown in the drawings, it should be understood that the disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
It should be noted that certain terms are used throughout the description and claims to refer to particular components. Those of skill in the art will understand that a person may refer to the same component by different names. The specification and claims do not identify differences in terms of components, but rather differences in terms of the functionality of the components. As used throughout the specification and claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. The description hereinafter sets forth the preferred embodiments for carrying out the present disclosure, but is not intended to limit the scope of the disclosure in general, as the description proceeds. The scope of the present disclosure is defined by the appended claims.
For the purposes of promoting an understanding of the embodiments of the disclosure, reference will now be made to the embodiments illustrated in the drawings and specific examples, without the intention of being limiting the embodiments of the disclosure.
In one embodiment, as shown in fig. 1, a method for preparing a novel ferroelectric ceramic includes the following steps:
s1: according to the stoichiometry Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ 229 and gPb are weighed respectively 3 O 4 、33.4g TiO 2 、24.4g ZrO 2 Mixing with 0.07g of MnO raw material to obtain a mixture;
s2: ball milling the mixture for 4 hours and then drying at 90 ℃;
s3: grinding the dried mixture, and sieving the mixture with a 60-mesh sieve to obtain mixed powder;
s4: presintering the mixed powder at 1250 ℃, preserving heat for 4 hours, and cooling to room temperature;
s5: grinding the mixed powder cooled to room temperature, continuously ball milling for 4 hours, and then drying at 90 ℃;
s6: secondary grinding is carried out on the dried mixed powder, PVA with the mass fraction of 8% is added for uniform mixing, and powder with the particle size of 0.15mm is screened out;
s7: the sieved powder is kept pressure for 90 seconds under 30MPa to obtain Pb ((Zr) with the stoichiometric formula 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Is a blank of a blank;
s8: stoichiometric Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ The blank is sintered at 950 ℃ for 4 hours and then cooled to room temperature, and the stoichiometric Pb ((Zr) is obtained 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Ferroelectric ceramics of (a);
s9: stoichiometric Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ The surface of the ferroelectric ceramic is polished smooth, silver paste is coated, and the surface is cooled to room temperature after heat preservation is carried out for 0.5 hour at 800 ℃;
s10: the stoichiometric amount of the silver paste which was cooled to room temperature was Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ The ferroelectric ceramic of (C) is kept at 430 ℃ for 20 hours.
In another embodiment, the present disclosure further provides a method for preparing a novel ferroelectric ceramic, including the steps of:
s1: according to the stoichiometry Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ 114.5 portions gPb portions are weighed 3 O 4 、16.7g TiO 2 、12.2g ZrO 2 Mixing with 0.035g of MnO raw material to obtain a mixed material;
s2: ball milling the mixture for 6 hours and then drying at 100 ℃;
s3: grinding the dried mixture, and sieving the mixture with a 60-mesh sieve to obtain mixed powder;
s4: presintering the mixed powder at 1300 ℃, preserving the heat for 6 hours, and cooling to room temperature;
s5: grinding the mixed powder cooled to room temperature, continuously ball milling for 6 hours, and then drying at 100 ℃;
s6: secondary grinding is carried out on the dried mixed powder, PVA with the mass fraction of 8% is added for uniform mixing, and powder with the particle size of 0.28mm is screened out;
s7: maintaining the pressure of the sieved powder for 100 seconds under the pressure of 30MPa to obtain Pb ((Zr) with the stoichiometric formula 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Is a blank of a blank;
s8: stoichiometric Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ The blank is sintered at 1000 ℃ for 6 hours and then cooled to room temperature, and the stoichiometric Pb ((Zr) is obtained 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Ferroelectric ceramics of (a);
s9: stoichiometric Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ The surface of the ferroelectric ceramic is polished smooth, silver paste is coated, and the surface is cooled to room temperature after heat preservation is carried out for 0.5 hour at 800 ℃;
s10: the stoichiometric amount of the silver paste which was cooled to room temperature was Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ The ferroelectric ceramic of (C) is kept at 450 ℃ for 20 hours.
The two examples are in the prior lead zirconate titanate Pb (Zr, ti) O 3 Doping in ferroelectric ceramicsAnd a proper amount of aliovalent element Mn is used for replacing lattice positions of Zr or Ti and introducing oxygen vacancies delta, so that a novel ferroelectric ceramic is formed. The doped aliovalent element Mn and oxygen vacancy delta form a defect dipole after heat preservation for 20 hours at the high temperature of 430-450 ℃, and the distribution of the defect dipole has the same structure as Pb (Zr, ti) O 3 The ferroelectric ceramic has the same domain structure, can provide a restoring force, so that the ferroelectric polarization reversed by the externally applied electric field can be restored to the initial state, thereby realizing the enhancement of the electric card effect of the existing ferroelectric ceramic.
The electrocaloric effect of the novel ferroelectric ceramics prepared by the above-described examples is described below by way of fig. 2 (a) through 4 (b).
Pb (Zr, ti) O in absence of defective dipole 3 In ferroelectric ceramics, in an initial state, as shown in fig. 2 (a), ferroelectric spontaneous polarization is completely randomly disordered; under the action of the applied electric field, the ferroelectric spontaneous polarization is oriented by the applied electric field, and the ferroelectric spontaneous polarization presents an orderly arranged state as shown in fig. 2 (b); after the applied electric field is removed, as shown in fig. 2 (c), the spontaneous polarization of the ferroelectric ceramic cannot be completely restored to the disordered state.
When in Pb (Zr, ti) O 3 Doping of the ferroelectric ceramic with an aliovalent element Mn and an oxygen vacancy delta to form a stoichiometric formula Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ After ferroelectric ceramics (abbreviated as PZTM), the aliovalent element Mn and oxygen vacancy delta are subjected to high-temperature heat preservation treatment to form a defect dipole, and a distribution state as shown in the figure 2 (d) (wherein, a solid arrow represents ferroelectric spontaneous polarization and a dotted arrow represents the defect dipole) which is the same as ferroelectric spontaneous polarization is generated; when an external electric field acts on the PZTM ferroelectric ceramic, the spontaneous polarization of the ferroelectric ceramic is oriented by the external electric field, the ferroelectric ceramic presents an ordered arrangement state as shown in a figure 2 (e), and the defect dipoles still keep the original distribution state unchanged; when the applied electric field is removed, the spontaneous polarization of the ferroelectric ceramic can be restored to the completely disordered arrangement state in the initial state as shown in fig. 2 (f) by the effect of the defective dipole restoring force.
As can be seen from comparing fig. 2 (c) with fig. 2 (f), the defect dipole is formed by the high temperature heat preservation treatment of the aliovalent element Mn and the oxygen vacancy δ, and the ferroelectric polarization distribution state can be changed much by the electric field effect, so as to generate a larger electric clamping effect.
Fig. 3 (a) shows the hysteresis loop of the PZTM ferroelectric ceramic without heat preservation. The PZTM ferroelectric ceramic without heat preservation as shown in FIG. 3 (a) shows typical single hysteresis loop characteristics and has a large remnant polarization at an applied electric field of 0, which is disadvantageous for the generation of large electric card effects in PZTM ceramics. It was also found that the ferroelectric hysteresis loop exhibited by the PZTM ferroelectric ceramic without heat preservation treatment has a stoichiometric formula of Pb (Zr) with the undoped Mn element 0.2 ，Ti 0.8 )O 3 The ferroelectric hysteresis loop of the ferroelectric ceramics has high similarity, so that the subsequent electric clamping effect obtained by testing the PZTM ferroelectric ceramics without heat preservation treatment can also react Pb (Zr) to a certain extent 0.2 ，Ti 0.8 )O 3 Electrocaloric effect in ferroelectric ceramics.
Fig. 3 (b) shows the hysteresis loop of the heat-insulated PZTM ferroelectric ceramic. The heat-preserved PZTM ferroelectric ceramic shown in fig. 3 (b) shows typical characteristics of double hysteresis loops, and when the applied electric field is 0, the remnant polarization is very small, that is, it is shown that defective dipoles with restoring force are generated in the heat-preserved PZTM ferroelectric ceramic, and the ferroelectric polarization oriented by the applied electric field can be restored to a disordered arrangement state.
Fig. 4 (a) and fig. 4 (b) are schematic diagrams of electrical card effects of the PZTM ferroelectric ceramic subjected to heat preservation treatment and not subjected to heat preservation treatment, respectively, wherein an upper right-hand insert diagram is a heat flow curve of the PZTM ferroelectric ceramic in the processes of applying an electric field and removing the electric field, a bar diagram is a temperature change of the PZTM ferroelectric ceramic calculated according to the heat flow curve, a grid filling column is a temperature increase of the PZTM ferroelectric ceramic caused by the applying the electric field, and a black filling column is a temperature decrease of the PZTM ferroelectric ceramic caused by the removing the electric field.
In fig. 4 (b), in the PZTM ferroelectric ceramic not subjected to the heat preservation process, the decrease in temperature of the ferroelectric ceramic caused by the de-electric field (black filled columns) is much smaller than the increase in temperature of the ferroelectric ceramic caused by the applied electric field (grid filled columns), and the decrease in temperature of the ferroelectric ceramic caused by the de-electric field in the second electric field cycle (0.1 ℃) is much smaller than the decrease in temperature of the ferroelectric ceramic caused by the de-electric field in the first electric field cycle (0.4 ℃). In fig. 4 (a), in the PZTM ferroelectric ceramic treated by the heat preservation process, the temperature decrease of the ferroelectric ceramic caused by the second de-electric field is equal to the temperature decrease of the ferroelectric ceramic caused by the first de-electric field, which is about 0.7 ℃.
The above results indicate that: after heat preservation treatment at high temperature, the defect dipole formed between Mn element and oxygen vacancy delta can obviously enhance the electric clamping effect of ferroelectric ceramic, so that the temperature change in the ferroelectric ceramic is greatly improved.
The foregoing has outlined rather broadly the principles and embodiments of the present disclosure using specific examples that are presented herein to aid in the understanding of the methods of the present disclosure and the core concepts thereof; meanwhile, as those skilled in the art will have variations in the specific embodiments and application scope in light of the ideas of the present disclosure, the present disclosure should not be construed as being limited to the above description.
Claims (8)
1. A preparation method of novel ferroelectric ceramics comprises the following steps:
s1: according to the stoichiometry Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Pb was weighed separately 3 O 4 、TiO 2 、ZrO 2 Mixing with MnO raw materials to obtain a mixture;
s2: ball milling and drying the mixture;
s3: grinding and sieving the dried mixture to obtain mixed powder;
s4: presintering the mixed powder, preserving heat and cooling to room temperature;
s5: grinding and drying the mixed powder cooled to room temperature;
s6: secondary grinding the dried mixed powder, adding PVA with the mass fraction of 8%, uniformly mixing, and sieving to obtain powder with the particle size of 0.15-0.28 mm;
s7: maintaining the pressure of the sieved powder to obtain Pb ((Zr) with the stoichiometric amount 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Is a blank of a blank;
s8: stoichiometric Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Cooling to room temperature after sintering the blank to obtain the stoichiometric Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Ferroelectric ceramics of (a);
s9: stoichiometric Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Polishing the surface of the ferroelectric ceramic, coating silver paste, preserving heat and cooling to room temperature;
s10: the stoichiometric amount of the silver paste which was cooled to room temperature was Pb ((Zr) 0.2 ，Ti 0.8 ) 0.99 ，Mn 0.01 )O 3-δ Is used for heat preservation of ferroelectric ceramics.
2. The method according to claim 1, wherein, preferably, in step S2, the mixture is ball milled for 4-6 hours.
3. The method according to claim 1, wherein in step S2, the mixture is dried at 90-100 ℃ after ball milling.
4. The method according to claim 1, wherein in step S4, the mixed powder is pre-fired at 1250-1300 ℃.
5. The method according to claim 1, wherein in step S7, the sieved powder is maintained at a pressure of 30MPa for 90-100 seconds.
6. The method according to claim 1, wherein in step S8, the green part sintering temperature is 950-1000 ℃.
7. The method according to claim 1, wherein in step S8, the green part is sintered for 4-6 hours.
8. The method according to claim 1, wherein in step S10, the ferroelectric ceramic cooled to room temperature and coated with silver paste is incubated at 430-450 ℃.
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