CN116065075A - Metal-relaxation ferroelectric ceramic with micro-nano composite structure and preparation method thereof - Google Patents
Metal-relaxation ferroelectric ceramic with micro-nano composite structure and preparation method thereof Download PDFInfo
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- 239000002184 metal Substances 0.000 claims abstract description 23
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- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims description 18
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- 238000007873 sieving Methods 0.000 claims description 6
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- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
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- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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Abstract
The invention relates to a metal-relaxation ferroelectric ceramic with a micro-nano composite structure and a preparation method thereof, belonging to the field of functional ceramic materials. The invention aims to solve the problem of low depolarization temperature of the existing BNT-based ceramic. The BNT-BKT/Ag ceramic with a micro-nano composite structure is prepared by controlling the sintering temperature and the heat preservation time, wherein metal silver particles with the size of 4-6 mu m are uniformly distributed in nano-scale ceramic grains as a composite body to form the micro-nano composite structure. The Ag particles have a larger stress effect on ceramic grains in the ceramic heating process, so that depolarization behavior of BNT-BKT ceramic is inhibited, and the bismuth sodium titanate-bismuth potassium titanate piezoelectric ceramic with high depolarization temperature is obtained.
Description
Technical Field
The invention belongs to the field of functional ceramic materials, and particularly relates to a metal-relaxation ferroelectric ceramic with a micro-nano composite structure and a preparation method thereof.
Background
Piezoelectric ceramics are commonly used in electromechanical conversion devices as a multifunctional material for performing mutual conversion between mechanical energy and electrical energy. In recent years, with the rising of ecological environmental awareness and the demand of society sustainable development strategy, the production and use of lead-based piezoelectric ceramics and related devices are limited, and the development and use of lead-free piezoelectric ferroelectric ceramics are developed. Bismuth sodium titanate (Bi) 0.5 Na 0.5 TiO 3 BNT) as a lead-free relaxor ferroelectric, not only has good ferroelectric properties, but also has a Curie temperature (T) comparable to lead-based ceramics m About 300 c) and thus lead-free BNT systems have attracted considerable attention.
The pure BNT system has low resistivity and high coercive field, so that ceramics are difficult to fully polarize, and the piezoelectric performance is not ideal. The piezoelectric constant d of BNT-based ceramics can be improved by constructing a three-party-four-party quasi-homotypic phase boundary (MPB) in a BNT-based system through multiple solid solutions 33 And a mechanical quality factor k p For example, the 0.94BNT-0.06BT and 0.80BNT-0.20BKT systems. However, BNT-based piezoceramics, due to the presence of ferroelectric-relaxation phase transitions, have a depolarization temperature T before the Curie temperature d This temperature is therefore a critical parameter in determining the actual temperature range in which the ceramic will be used. Recently, it has been found that quenching treatments can raise the depolarization temperature of BNT-based ceramics; however, the sample is liable to crack or even break due to extremely high temperature during quenching, resulting in difficulty in obtaining a complete and large ceramic sheet. Therefore, developing a novel and stable preparation method for improving the depolarization temperature of BNT-based ceramics has extremely important research value and practical significance.
Disclosure of Invention
The invention aims to solve the problem of low depolarization temperature of the existing BNT-based ceramic, and provides a metal-relaxor ferroelectric ceramic with a micro-nano composite structure and a preparation method thereof.
A metal-relaxation ferroelectric ceramic with micro-nano composite structure is a micro-nano grain composite structure formed by uniformly distributing metal Ag particles of 4-6 μm in the middle of nano BNT-BKT ceramic grains.
The preparation method of the metal-relaxation ferroelectric ceramic with the micro-nano composite structure is completed by the following steps:
1. according to 0.8Bi 0.5 Na 0.5 TiO 3 -0.2Bi 0.5 K 0.5 TiO 3 Proportioning and weighing Bi 2 O 3 、Na 2 CO 3 、K 2 CO 3 And TiO 2 Bi to be weighed 2 O 3 、Na 2 CO 3 、K 2 CO 3 And TiO 2 Mixing and placing the materials in a ball milling tank, performing ball milling by taking absolute ethyl alcohol as a ball milling medium, and drying wet materials after ball milling to obtain a dry mixture; grinding the dried mixture by using a mortar to obtain mixture powder, loading the mixture powder into a corundum crucible, and then placing the corundum crucible into a box furnace for calcination to obtain BNT-BKT pre-sintered powder with a pure perovskite structure;
2. pre-sintering BNT-BKT powder with pure perovskite structure and silver oxide Ag 2 The O powder is weighed according to the mol ratio of 1 (0.025-0.125), and the weighed BNT-BKT presintered powder with a pure perovskite structure and silver oxide Ag are mixed 2 Mixing and grinding O powder in a mortar to obtain mixed powder;
3. adding an adhesive into the mixed powder, grinding uniformly, sieving and pressing into a wafer;
4. placing the three formed discs in a crucible paved with platinum sheets in a stacking way, and arranging adhesive for 2-4 hours at 500-650 ℃; then sintering is carried out at the temperature of 1100-1200 ℃ for 1-4 hours; the metal silver forms a liquid phase at the melting point of 962 ℃, and is uniformly distributed in the middle of BNT-BKT ceramic grains after flowing and aggregation to obtain a metal silver composite sodium bismuth titanate-potassium bismuth titanate ceramic sheet;
5. and (3) plating gold on the metal silver composite bismuth sodium titanate-bismuth potassium titanate ceramic sheet by using a small metal sputtering coating machine, carrying out polarization treatment on the ceramic sheet by adopting a direct-current high-voltage power supply, and obtaining the metal silver composite bismuth sodium titanate-bismuth potassium titanate piezoelectric ceramic after polarization is completed.
The invention has the beneficial effects that: the BNT-BKT/Ag ceramic with a micro-nano composite structure is prepared by controlling the sintering temperature and the heat preservation time, wherein metal silver particles with the size of 4-6 mu m are uniformly distributed in nano-scale ceramic grains as a composite body to form the micro-nano composite structure. The large thermal expansion coefficient and the large-size Ag particles exert stress on the nano-scale ceramic grains in the ceramic heating process, so that the depolarization temperature of BNT-BKT ceramic is improved; its depolarization temperature T d 170-185 ℃ which is 35-50 ℃ higher than BNT-BKT ceramics.
Drawings
FIG. 1 is an XRD pattern for BNT-BKT/xAg (x= 0,0.15) ceramic;
FIG. 2 is a surface SEM image of BNT-BKT/0.15Ag ceramic;
FIG. 3 is an elemental surface scan spectrum of Ag in BNT-BKT/0.15Ag ceramic;
FIG. 4 is a graph showing the room temperature hysteresis loop of BNT-BKT/0.15Ag ceramic;
FIG. 5 is a dielectric temperature spectrum of 0.80BNT-0.20BKT ceramic; wherein 1 represents a frequency of 1kHz,2 represents a frequency of 10kHz, and 3 represents a frequency of 100kHz;
FIG. 6 is a dielectric temperature spectrum of BNT-BKT/0.15Ag ceramic; wherein 1 denotes a frequency of 1kHz,2 denotes a frequency of 10kHz, and 3 denotes a frequency of 100kHz.
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, but also includes any combination of the specific embodiments.
The first embodiment is as follows: the metal-relaxation ferroelectric ceramic with the micro-nano composite structure is a micro-nano grain composite structure formed by uniformly distributing metal Ag particles with the diameter of 4-6 mu m in the middle of nano BNT-BKT ceramic grains.
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: the chemical general formula of the metal-relaxation ferroelectric ceramic with the micro-nano composite structure is 0.8Bi 0.5 Na 0.5 TiO 3 -0.2Bi 0.5 K 0.5 TiO 3 And (2) xAg, namely BNT-BKT/xAg, wherein x is the molar ratio of Ag to BNT-BKT, and x is more than or equal to 0.05 and less than or equal to 0.25. The other is the same as in the first embodiment.
And a third specific embodiment: the preparation method of the metal-relaxation ferroelectric ceramic with the micro-nano composite structure is completed by the following steps:
1. according to 0.8Bi 0.5 Na 0.5 TiO 3 -0.2Bi 0.5 K 0.5 TiO 3 Proportioning and weighing Bi 2 O 3 、Na 2 CO 3 、K 2 CO 3 And TiO 2 Bi to be weighed 2 O 3 、Na 2 CO 3 、K 2 CO 3 And TiO 2 Mixing and placing the materials in a ball milling tank, performing ball milling by taking absolute ethyl alcohol as a ball milling medium, and drying wet materials after ball milling to obtain a dry mixture; grinding the dried mixture by using a mortar to obtain mixture powder, loading the mixture powder into a corundum crucible, and then placing the corundum crucible into a box furnace for calcination to obtain BNT-BKT pre-sintered powder with a pure perovskite structure;
2. pre-sintering BNT-BKT powder with pure perovskite structure and silver oxide Ag 2 O powder is weighed according to the mol ratio of 1:0.025-0.125, and the weighed BNT-BKT presintered powder with a pure perovskite structure and silver oxide Ag are mixed 2 Mixing and grinding O powder in a mortar to obtain mixed powder;
3. adding an adhesive into the mixed powder, grinding uniformly, sieving and pressing into a wafer;
4. placing the three formed discs in a crucible paved with platinum sheets in a stacking way, and arranging adhesive for 2-4 hours at 500-650 ℃; then sintering is carried out at the temperature of 1100-1200 ℃ for 1-4 hours; the metal silver forms a liquid phase at the melting point of 962 ℃, and is uniformly distributed in the middle of BNT-BKT ceramic grains after flowing and aggregation to obtain a metal silver composite sodium bismuth titanate-potassium bismuth titanate ceramic sheet;
5. and (3) plating gold on the metal silver composite bismuth sodium titanate-bismuth potassium titanate ceramic sheet by using a small metal sputtering coating machine, carrying out polarization treatment on the ceramic sheet by adopting a direct-current high-voltage power supply, and obtaining the metal silver composite bismuth sodium titanate-bismuth potassium titanate piezoelectric ceramic after polarization is completed.
Depolarization temperature test is carried out on the metallic silver composite bismuth sodium titanate-bismuth potassium titanate piezoelectric ceramic prepared in the embodiment: the polarized metallic silver composite sodium bismuth titanate-potassium bismuth titanate ceramic sheet is placed into a dielectric temperature spectrum tester, and dielectric properties of the sheet are tested within the temperature range of 20-450 ℃ to determine the depolarization temperature of BNT-BKT/Ag ceramic.
The specific embodiment IV is as follows: the third difference between this embodiment and the third embodiment is that: parameters of the ball milling in step one: the ball-material ratio is (1.2-1.5), 1, the rotating speed is 180-230 rpm, and the ball milling time is 24-48 h; the temperature of the drying is 80-130 ℃. The other is the same as in the third embodiment.
Fifth embodiment: this embodiment differs from the third or fourth embodiment in that: parameters of the calcination in step one: the calcination temperature is 800-900 ℃, the temperature rising rate is 2-10 ℃/min, and the calcination time is 2-6 h. The other is the same as in the third or fourth embodiment.
Specific embodiment six: this embodiment differs from one of the third to fifth embodiments in that: and step two, mixing and grinding, namely adding absolute ethyl alcohol according to the mass ratio of 1 (1.2-1.5), grinding for 10-30 min by hand, and adding the same amount of absolute ethyl alcohol again after the alcohol is evaporated and dried, and grinding until the alcohol is completely evaporated. The others are the same as in one of the third to fifth embodiments.
The mass ratio is BNT-BKT presintered powder with pure perovskite structure and silver oxide Ag 2 The mass ratio of the total mass of the O powder to the absolute ethyl alcohol is 1 (1.2-1.5).
Seventh embodiment: this embodiment differs from one of the third to sixth embodiments in that: in the third step, the binder is PVA, and the addition amount of the binder is 7% of the mass of the mixed powder. The others are the same as in one of the third to sixth embodiments.
Eighth embodiment: this embodiment differs from one of the third to seventh embodiments in that: the mesh number of the screening in the third step is 80-120 meshes; the pressed wafer is pressed into a wafer under the pressure of 4-8 MPa. The others are the same as in one of the third to seventh embodiments.
Detailed description nine: this embodiment differs from one of the third to eighth embodiments in that: and step four, the temperature rising rate of sintering is 2-6 ℃/min, and the temperature reducing rate is 4-10 ℃/min. The others are the same as in one of the third to eighth embodiments.
Detailed description ten: this embodiment differs from one of the third to ninth embodiments in that: and step four, covering two layers of crucibles on the stacked and formed wafers. The others are the same as in one of the third to ninth embodiments.
The present embodiment can reduce volatilization of elements.
Eleventh embodiment: this embodiment differs from one of the third to tenth embodiments in that: in the fifth step, the gold plating time is 5-15 min; the electric field intensity of the polarization treatment is 30-70 kV/cm, and the polarization time is 30-60 min. The others are the same as in one of the third to tenth embodiments.
Twelve specific embodiments: this embodiment differs from one of the third to eleventh embodiments in that: and step five, the diameter of Ag particles in the metal silver composite bismuth sodium titanate-bismuth potassium titanate piezoelectric ceramic is 4-6 mu m, and the grain size of BNT-BKT ceramic is 300-600 nm. The others are the same as in one of the third to eleventh embodiments.
The following examples are used to verify the benefits of the present invention:
embodiment one:
the preparation method of the metal-relaxation ferroelectric ceramic with the micro-nano composite structure is completed by the following steps:
1. according to 0.8Bi 0.5 Na 0.5 TiO 3 -0.2Bi 0.5 K 0.5 TiO 3 Proportioning and weighing Bi 2 O 3 、Na 2 CO 3 、K 2 CO 3 And TiO 2 Bi to be weighed 2 O 3 、Na 2 CO 3 、K 2 CO 3 And TiO 2 Mixing, adding absolute ethyl alcohol according to a mass ratio of 1:1.3, placing the mixture into a ball milling tank, ball milling the mixture for 30 hours by adopting a ball mill under the condition that the rotating speed is 200 rpm, and drying the wet material after ball milling at 110 ℃ to obtain a dry mixture; grinding the dried mixture by using a mortar to obtain mixture powder, placing the mixture powder into a corundum crucible, then placing the corundum crucible into a box-type furnace, calcining the corundum crucible for 4 hours at 830 ℃, and obtaining BNT-BKT pre-sintered powder with a pure perovskite structure at a heating rate of 5 ℃/min;
2. pre-sintering BNT-BKT powder with pure perovskite structure and silver oxide Ag 2 O powder is weighed according to the mol ratio of 1:0.075, and the weighed BNT-BKT presintered powder with a pure perovskite structure and silver oxide Ag are mixed 2 Placing O powder into a mortar, adding absolute ethyl alcohol according to the mass ratio of 1:1.3, grinding for 15 minutes until the alcohol is completely evaporated, adding absolute ethyl alcohol again according to the same mass ratio, grinding until the alcohol is evaporated and dried, and obtaining mixed powder;
3. adding an adhesive into the mixed powder, grinding uniformly, sieving with a 80-mesh sieve, and pressing into a wafer with the diameter of 10mm under the pressure of 6MPa, wherein pressure maintaining is not needed; the adhesive is PVA, and the addition amount of the adhesive is 7% of the mass of the mixed powder;
4. placing the three formed discs in a crucible with platinum sheets, covering two layers of crucibles to reduce element volatilization, discharging adhesive at 550deg.C for 3 hr, and ensuring Ag 2 O is completely divided into Ag and O 2 The method comprises the steps of carrying out a first treatment on the surface of the Then sintering is carried out at 1120 ℃, the heat preservation time is 1h, the heating rate is 2 ℃/min, and the cooling rate is 4 ℃/min; the metallic silver forms a liquid phase at the melting point of 962 ℃, and is uniformly distributed in the middle of BNT-BKT ceramic grains after flowing and aggregation to obtain the BNT-BKT/0.15Ag ceramic sheet.
Comparative examples:
the preparation method of the metal-relaxation ferroelectric ceramic with the micro-nano composite structure is completed by the following steps:
1. according to 0.8Bi 0.5 Na 0.5 TiO 3 -0.2Bi 0.5 K 0.5 TiO 3 Proportioning and weighing Bi 2 O 3 、Na 2 CO 3 、K 2 CO 3 And TiO 2 Bi to be weighed 2 O 3 、Na 2 CO 3 、K 2 CO 3 And TiO 2 Mixing, adding absolute ethyl alcohol according to a mass ratio of 1:1.3, placing the mixture into a ball milling tank, ball milling the mixture for 30 hours by adopting a ball mill under the condition that the rotating speed is 200 rpm, and drying the wet material after ball milling at 110 ℃ to obtain a dry mixture; grinding the dried mixture by using a mortar to obtain mixture powder, placing the mixture powder into a corundum crucible, then placing the corundum crucible into a box-type furnace, calcining the corundum crucible for 4 hours at 830 ℃, and obtaining BNT-BKT pre-sintered powder with a pure perovskite structure at a heating rate of 5 ℃/min;
2. adding BNT-BKT presintered powder with a pure perovskite structure into a mortar, adding absolute ethyl alcohol according to a mass ratio of 1:1.3, grinding for 15 minutes until alcohol is completely evaporated, adding absolute ethyl alcohol again according to the same mass ratio, grinding until alcohol is evaporated and dried, and obtaining mixed powder;
3. adding an adhesive into the mixed powder, grinding uniformly, sieving with a 80-mesh sieve, and pressing into a wafer with the diameter of 10mm under the pressure of 6MPa, wherein pressure maintaining is not needed; the adhesive is PVA, and the addition amount of the adhesive is 7% of the mass of the mixed powder;
4. placing the three formed discs in a crucible paved with platinum sheets in a stacking way, covering two layers of crucibles on the three formed discs to reduce element volatilization, and arranging an adhesive for 2 hours at 550 ℃; then sintering is carried out at 1160 ℃, the heat preservation time is 2 hours, the heating rate is 3 ℃/min, and the cooling rate is 5 ℃/min; obtaining the 0.80BNT-0.20BKT ceramic plate.
The ceramics of example one and comparative examples were ground to a fine powder and tested for X-ray diffraction patterns at room temperature. As shown in fig. 1, the x=0 sample has a pure perovskite structure, and the x=0.15 sample has a second phase of a small amount of metallic Ag, which is integrally represented as a complex phase of perovskite and metallic Ag. In addition, the two are in pseudo-cubic phases in the unpolarized state.
After sputtering gold electrode on BNT-BKT/0.15Ag ceramic sample surface, observing the appearance of ceramic surface by using a scanning electron microscope, and performing element scanning detection, as shown in FIG. 2 and FIG. 3. The composite structure of larger micron-sized particles and nano-sized grains appears in the morphology graph, the particle with the size of 4-6 mu m is determined to be metal Ag through an element surface scanning spectrum, the size of BNT-BKT ceramic grains is 300-600 nm, the Ag particles can be uniformly distributed in the ceramic grains, and the micro-nano composite structure is formed.
Ferroelectric properties were tested on BNT-BKT/0.15Ag ceramics. The hysteresis loop was tested at room temperature at a frequency of 1Hz with an electric field strength of 60kV/cm, as shown in FIG. 4. BNT-BKT/0.15Ag ceramic exhibits a typical saturated electric hysteresis loop shape, coercive electric field Ec of 35kV/cm, residual polarization strength Pr of 26. Mu.C/cm 2 Indicating that the ceramic is ferroelectric.
And (3) carrying out polarization treatment on the ceramic plate for 30min by using a direct-current high-voltage power supply at room temperature and a 50kV/cm electric field after sputtering the gold electrode in the first embodiment and the comparative embodiment, and obtaining the polarized BNT-BKT/xAg (x= 0,0.15) piezoelectric ceramic after polarization.
And carrying out dielectric temperature spectrum test on the BNT-BKT/xAg ceramic plate obtained by polarization. Dielectric constants and dielectric losses at different temperatures were measured at different test frequencies, wherein FIG. 5 is a dielectric temperature spectrum of BNT-BKT ceramic and FIG. 6 is a dielectric temperature spectrum of BNT-BKT/0.15Ag ceramic. Firstly, the phenomena of frequency dispersion and temperature dispersion appear in the two ceramics, which indicates that the two ceramics are relaxation ferroelectric ceramics; and the BNT-BKT/0.15Ag ceramic low temperature region has lower frequency dispersion degree than BNT-BKT ceramic. Secondly, the first dielectric abnormal peak of BNT-BKT ceramic is T d A peak indicating that the depolarization temperature of the ceramic is 136 ℃; BNT-BKT/T of 0.15Ag ceramic d The peak was around 179℃which is 43℃higher than that of BNT-BKT ceramics.
Claims (10)
1. The metal-relaxor ferroelectric ceramic with the micro-nano composite structure is characterized in that the metal-relaxor ferroelectric ceramic with the micro-nano composite structure is a micro-nano grain composite structure formed by uniformly distributing metal Ag particles of 4-6 mu m in the middle of nano BNT-BKT ceramic grains.
2. According to the weightsA metal-relaxor ferroelectric ceramic having a micro-nano composite structure as claimed in claim 1, wherein the metal-relaxor ferroelectric ceramic having a micro-nano composite structure has a chemical formula of 0.8Bi 0.5 Na 0.5 TiO 3 -0.2Bi 0.5 K 0.5 TiO 3 And (2) xAg, namely BNT-BKT/xAg, wherein x is the molar ratio of Ag to BNT-BKT, and x is more than or equal to 0.05 and less than or equal to 0.25.
3. The method for preparing a metal-relaxor ferroelectric ceramic having a micro-nano composite structure as set forth in claim 1, wherein the method for preparing the metal-relaxor ferroelectric ceramic having the micro-nano composite structure is accomplished by the steps of:
1. according to 0.8Bi 0.5 Na 0.5 TiO 3 -0.2Bi 0.5 K 0.5 TiO 3 Proportioning and weighing Bi 2 O 3 、Na 2 CO 3 、K 2 CO 3 And TiO 2 Bi to be weighed 2 O 3 、Na 2 CO 3 、K 2 CO 3 And TiO 2 Mixing and placing the materials in a ball milling tank, performing ball milling by taking absolute ethyl alcohol as a ball milling medium, and drying wet materials after ball milling to obtain a dry mixture; grinding the dried mixture by using a mortar to obtain mixture powder, loading the mixture powder into a corundum crucible, and then placing the corundum crucible into a box furnace for calcination to obtain BNT-BKT pre-sintered powder with a pure perovskite structure;
2. pre-sintering BNT-BKT powder with pure perovskite structure and silver oxide Ag 2 The O powder is weighed according to the mol ratio of 1 (0.025-0.125), and the weighed BNT-BKT presintered powder with a pure perovskite structure and silver oxide Ag are mixed 2 Mixing and grinding O powder in a mortar to obtain mixed powder;
3. adding an adhesive into the mixed powder, grinding uniformly, sieving and pressing into a wafer;
4. placing the three formed discs in a crucible paved with platinum sheets in a stacking way, and arranging adhesive for 2-4 hours at 500-650 ℃; then sintering is carried out at the temperature of 1100-1200 ℃ for 1-4 hours; the metal silver forms a liquid phase at the melting point of 962 ℃, and is uniformly distributed in the middle of BNT-BKT ceramic grains after flowing and aggregation to obtain a metal silver composite sodium bismuth titanate-potassium bismuth titanate ceramic sheet;
5. and (3) plating gold on the metal silver composite bismuth sodium titanate-bismuth potassium titanate ceramic sheet by using a small metal sputtering coating machine, carrying out polarization treatment on the ceramic sheet by adopting a direct-current high-voltage power supply, and obtaining the metal silver composite bismuth sodium titanate-bismuth potassium titanate piezoelectric ceramic after polarization is completed.
4. A method for preparing a metal-relaxor ferroelectric ceramic having a micro-nano composite structure as set forth in claim 3, wherein the parameters of the ball milling in the first step: the ball-material ratio is (1.2-1.5), 1, the rotating speed is 180-230 rpm, and the ball milling time is 24-48 h; the temperature of the drying is 80-130 ℃.
5. A method for producing a metal-relaxor ferroelectric ceramic having a micro-nano composite structure as claimed in claim 3, wherein the parameters of the calcination in the first step are as follows: the calcination temperature is 800-900 ℃, the temperature rising rate is 2-10 ℃/min, and the calcination time is 2-6 h.
6. The method for preparing metal-relaxor ferroelectric ceramic with micro-nano composite structure according to claim 3, wherein in the second step, the mixed grinding is carried out by adding absolute ethyl alcohol into the mixture according to mass ratio of 1 (1.2-1.5), hand grinding for 10-30 min, evaporating and drying alcohol, adding the same absolute ethyl alcohol again, and grinding until alcohol is evaporated.
7. The method for preparing a metal-relaxor ferroelectric ceramic having a micro-nano composite structure as set forth in claim 3, wherein the binder in the third step is PVA, and the amount of the binder added is 7% of the mass of the mixed powder.
8. The method for producing a metal-relaxor ferroelectric ceramic having a micro-nano composite structure as claimed in claim 3, wherein the mesh number of the sieving in the third step is 80 to 120 mesh; the pressed wafer is pressed into a wafer under the pressure of 4-8 MPa.
9. The method for preparing a metal-relaxor ferroelectric ceramic having a micro-nano composite structure as set forth in claim 3, wherein the gold plating time in the fifth step is 5 to 15 minutes; the electric field intensity of the polarization treatment is 30-70 kV/cm, and the polarization time is 30-60 min.
10. The method for preparing metal-relaxor ferroelectric ceramic with micro-nano composite structure according to claim 3, wherein the Ag particle diameter in the metal silver composite bismuth sodium titanate-bismuth potassium titanate piezoelectric ceramic in the fifth step is 4-6 μm, and the BNT-BKT ceramic grain size is 300-600 nm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11219826A (en) * | 1998-02-02 | 1999-08-10 | Mitsubishi Materials Corp | Magnetic dielectric compound porcelain |
| CN101028979A (en) * | 2006-02-27 | 2007-09-05 | 西北工业大学 | Lead-free piezoelectric knitting ceramic of titanic acid bismuth sodium-titanic acid bismuth potassium and its production |
| US20140368090A1 (en) * | 2011-12-20 | 2014-12-18 | Taiyo Yuden Co., Ltd. | Piezoelectric device and piezoelectric ceramic composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11219826A (en) * | 1998-02-02 | 1999-08-10 | Mitsubishi Materials Corp | Magnetic dielectric compound porcelain |
| CN101028979A (en) * | 2006-02-27 | 2007-09-05 | 西北工业大学 | Lead-free piezoelectric knitting ceramic of titanic acid bismuth sodium-titanic acid bismuth potassium and its production |
| US20140368090A1 (en) * | 2011-12-20 | 2014-12-18 | Taiyo Yuden Co., Ltd. | Piezoelectric device and piezoelectric ceramic composition |
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