CN116120054B - Bismuth calcium titanate-based piezoelectric ceramic material and preparation method thereof - Google Patents
Bismuth calcium titanate-based piezoelectric ceramic material and preparation method thereof Download PDFInfo
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- CN116120054B CN116120054B CN202310108403.7A CN202310108403A CN116120054B CN 116120054 B CN116120054 B CN 116120054B CN 202310108403 A CN202310108403 A CN 202310108403A CN 116120054 B CN116120054 B CN 116120054B
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 40
- PMVFCJGPQOWMTE-UHFFFAOYSA-N bismuth calcium Chemical compound [Ca].[Bi] PMVFCJGPQOWMTE-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000919 ceramic Substances 0.000 claims abstract description 27
- -1 cerium ions Chemical class 0.000 claims abstract description 11
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 5
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 5
- 229910001460 tantalum ion Inorganic materials 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims description 26
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 24
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 24
- 238000005245 sintering Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 239000010936 titanium Substances 0.000 claims description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 229920002545 silicone oil Polymers 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 8
- 239000000853 adhesive Substances 0.000 claims description 8
- 230000001070 adhesive effect Effects 0.000 claims description 8
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 8
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 239000002612 dispersion medium Substances 0.000 claims description 8
- 230000005684 electric field Effects 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 8
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 8
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 8
- 230000010287 polarization Effects 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Chemical compound O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 8
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 8
- 229940075624 ytterbium oxide Drugs 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- 239000010955 niobium Substances 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 7
- 239000004677 Nylon Substances 0.000 description 6
- 229920001778 nylon Polymers 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 2
- 230000028161 membrane depolarization Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- ZYCNQNXMWCTETO-UHFFFAOYSA-N calcium oxygen(2-) yttrium(3+) borate Chemical compound [O-2].[Y+3].B([O-])([O-])[O-].[Ca+2] ZYCNQNXMWCTETO-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 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
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
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Abstract
The invention discloses a bismuth calcium titanate-based piezoelectric ceramic material and a preparation method thereof, wherein the ceramic material is doped with cerium ions at A site, ytterbium ions and tantalum ions at B site of CBT ceramic, and simultaneously is doped with Nb 2 O 5 Modifying; the stoichiometric amount is CaCe x Bi 4‑x Ti 4‑y (Yb 1/2 Ta 1/2 ) y O 15 +z mol％Nb 2 O 5 Wherein x is more than 0 and less than or equal to 0.1, y is more than 0 and less than or equal to 0.1, and z is more than 0 and less than or equal to 4. The ceramic material has the advantages of large piezoelectric constant, high Curie temperature and high-temperature resistivity, has practical application value in the field of high-temperature piezoelectric sensors, and is simple and stable in preparation process, convenient to operate and suitable for popularization of large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of piezoelectric ceramics, in particular to a bismuth calcium titanate-based piezoelectric ceramic material and a preparation method thereof.
Background
The industries such as automobiles, aerospace, energy sources and the like have urgent demands for high-temperature piezoelectric acceleration sensors. The core element of the high-temperature piezoelectric device is a piezoelectric material, and the quality of the device is determined by the quality of the material, so that the research on the high-temperature piezoelectric material is very important.
The piezoelectric material comprises piezoelectric monocrystal and ceramic material, and lead zirconate titanate, namely PZT-based ceramic, has been developed for decades, and the piezoelectric constant has been greatly improved, but the Curie temperature T c The temperature is lower than or equal to 400 ℃ and is lower than 300 ℃; lithium niobate (LiNbO) 3 )、Sr 2 Nb 2 O 7 、La 2 Ti 2 O 7 Lanthanum gallium silicate (La) 3 Ga 5 SiO 14 ) Monocrystalline materials such as calcium yttrium oxide borate (YCOB) and the like have extremely high Curie point (T) c The temperature is higher than 1000 ℃ and the high-temperature resistivity, but the piezoelectric constant is low, the technical development difficulty is high, the preparation cost is high, and the industrial large-scale application is difficult to realize.
The bismuth layered structure ceramic has higher Curie temperature, such as bismuth calcium titanate CaBi 4 Ti 4 O 15 The (CBT) system ceramic has a high curie temperature (780 ℃) but also has disadvantages such as a low piezoelectric constant (d) 33 =7.5 pC/N) and low high temperature resistivity (7×10 5 Omega cm@600℃). Therefore, improving the piezoelectric performance and the high-temperature resistivity of the bismuth calcium titanate-based piezoelectric ceramic material while maintaining a relatively high curie temperature is regarded as an important subject in the field of high-temperature material research.
Disclosure of Invention
Aiming at overcoming the defects in the prior art, the invention provides the bismuth calcium titanate-based piezoelectric ceramic material and the preparation method thereof, wherein the bismuth calcium titanate-based piezoelectric ceramic material has the advantages of large piezoelectric constant, high Curie temperature and high-temperature resistivity, and has practical application value in the field of high-temperature piezoelectric sensors.
To solve the above problems, an embodiment of the present invention provides in a first aspect a bismuth calcium titanate-based piezoelectric ceramic material in which cerium ions are doped at the A-site, ytterbium ions are doped at the B-site, and tantalum ions are doped at the B-site, while Nb is doped at the same time 2 O 5 Modifying;
the stoichiometric amount is CaCe x Bi 4-x Ti 4-y (Yb 1/2 Ta 1/2 ) y O 15 +z mol％Nb 2 O 5 Wherein x is more than 0 and less than or equal to 0.1,0＜y≤0.1，0＜z≤4。
according to the bismuth calcium titanate-based piezoelectric ceramic material provided by the embodiment of the invention, cerium ions are doped at the A site of CBT ceramic, ytterbium ions and tantalum ions are doped at the B site of CBT ceramic, and Nb is doped at the same time 2 O 5 Modification is performed so that the bismuth calcium titanate-based piezoelectric ceramic material maintains a high curie temperature (790 ℃) and a piezoelectric constant (from 7.5pC/N to 22 pC/N) and a high temperature resistivity (7×10) 5 The temperature of the mixture is increased to 4.5X10 ℃ at the temperature of Ω cm@600 DEG C 6 Greatly improves the temperature of omega cm@600℃.
In a second aspect, the embodiment of the invention provides a preparation method of the bismuth calcium titanate-based piezoelectric ceramic material, which comprises the following steps:
step 1, weighing various raw materials according to stoichiometric weighing, mixing, ball grinding into slurry, drying the slurry, and presintering to obtain presintered powder;
step 2, after secondary ball milling of the presintered powder, drying, adding an adhesive for grinding and granulating, sieving, and pressing and forming to obtain a thin round blank;
step 3, discharging glue from the thin round blank, and sintering to obtain a sintered ceramic sheet;
and 4, polishing and printing electrodes on two sides of the sintered ceramic sheet, sintering the electrodes, and placing the electrodes in silicone oil to apply voltage for polarization to obtain the bismuth calcium titanate-based piezoelectric ceramic material.
According to the embodiment of the invention, the method can be prepared by adopting a traditional solid-phase reaction method, has simple and stable preparation process and convenient operation, is suitable for popularization of large-scale industrial production, and has practical application value and wide application prospect.
Optionally, in step 1, the raw material comprises calcium carbonate CaCO 3 Bismuth oxide Bi 2 O 3 Titanium oxide Ti 2 O 3 CeO of cerium oxide 2 Ytterbium oxide Yb 2 O 3 Tantalum pentoxide Ta 2 O 5 And niobium pentoxide Nb 2 O 5 。
Optionally, in the step 1, during ball milling, absolute ethyl alcohol is used as a dispersion medium, and a planetary mill machine is used for mixed ball milling for 6-12 hours, and the rotating speed is 200-300 rpm; during drying, the slurry is dried at the temperature of 100-120 ℃; and (3) presintering at 650-750 ℃ during presintering, and preserving heat for 2-4 hours to obtain presintering powder.
Optionally, in the step 2, the time of the secondary ball milling is 12-24 hours.
Optionally, in step 2, the binder is a polyvinyl alcohol PVA aqueous solution with a mass ratio of 12%.
Optionally, in the step 2, after passing through a 60-mesh sieve, a thin round blank with the diameter of 12-15 mm and the thickness of 0.5-1 mm is pressed.
Optionally, in the step 3, the glue is discharged by preserving heat for 1h at 600-850 ℃; sintering is to sinter the thin round billet for 2 to 4 hours at 1050 to 1180 ℃.
Optionally, in step 4, a platinum/gold electrode is printed on the sintered ceramic plate polished on both sides, and then the electrode is sintered at 800-1000 ℃ and kept for 10-30 min.
Optionally, in the step 4, a direct current electric field of 12 kV/mm-15 kV/mm is applied to silicone oil at 200-240 ℃ for 20-40 min.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
FIG. 1 is a dielectric thermogram of a bismuth calcium titanate based piezoelectric ceramic material according to example 1 of the present invention;
FIG. 2 shows a bismuth calcium titanate-based piezoelectric ceramic material d according to examples 1 to 3 of the present invention 33 Graph of the values as a function of depolarization temperature.
Detailed Description
The technical scheme of the invention is described below through specific examples. It is to be understood that the mention of one or more method steps of the present invention does not exclude the presence of other method steps before and after the combination step or that other method steps may be interposed between these explicitly mentioned steps; it should also be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Moreover, unless otherwise indicated, the numbering of the method steps is merely a convenient tool for identifying the method steps and is not intended to limit the order of arrangement of the method steps or to limit the scope of the invention in which the invention may be practiced, as such changes or modifications in their relative relationships may be regarded as within the scope of the invention without substantial modification to the technical matter.
In order to better understand the above technical solution, exemplary embodiments of the present invention are described in more detail below. While exemplary embodiments of the invention are shown, it should be understood that the invention 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 invention to those skilled in the art.
The test materials adopted by the invention are all common commercial products and can be purchased in the market.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not limiting in any way.
Example 1
The stoichiometric formula of the bismuth calcium titanate-based piezoelectric ceramic material is as follows: caCe (CaCe) x Bi 4-x Ti 4-y (Yb 1/2 Ta 1/2 ) y O 15 +z mol％Nb 2 O 5 Where x=0.05, y=0.05, z=2.
Preparation of bismuth calcium titanate-based piezoelectric ceramic material:
step 1, weighing various raw materials (calcium carbonate CaCO) according to the stoichiometric amount 3 Bismuth oxide Bi 2 O 3 Titanium oxide Ti 2 O 3 CeO of cerium oxide 2 Ytterbium oxide Yb 2 O 3 Tantalum pentoxide Ta 2 O 5 And niobium pentoxide Nb 2 O 5 ) Placing the mixture into a nylon ball milling tank, taking absolute ethyl alcohol as a dispersion medium, mixing and ball milling for 6 hours by using a planetary mill machine with the total mass ratio of the absolute ethyl alcohol to the raw materials being 2:1, drying the slurry at 120 ℃ at the rotating speed of 300rpm, presintering at 750 ℃, and preserving the heat for 4 hours to obtain presintered powder.
And 2, performing secondary ball milling on the presintered powder for 24 hours, taking out and drying, adding PVA aqueous solution with the mass fraction of 5wt% as an adhesive, wherein the mass of the PVA aqueous solution is 12% of the total mass, grinding uniformly, sieving by a 60-mesh sieve, and pressing into a thin round billet with the diameter of 14mm and the thickness of 0.5mm by using 100 MPa.
And 3, discharging PVA solution from the thin round blank after heat preservation for 1h at 600 ℃, and then sintering the round blank for 3h at 1110 ℃ to obtain the sintered ceramic sheet.
And 4, polishing two sides of the sintered ceramic sheet after sintering, printing a platinum electrode, sintering the electrode at 800 ℃, preserving heat for 30min, and placing the electrode in 220 ℃ silicone oil, applying a direct current electric field of 15kV/mm, and maintaining for 30min for polarization.
The piezoelectric properties of the bismuth calcium titanate-based piezoelectric ceramic material obtained in the embodiment are as follows: d, d 33 =22pc/N, dielectric loss tan δ=0.10%, curie temperature T c =790 ℃, 600 ℃ resistivity 4.5×10 6 Ω·cm。
Example 2
The stoichiometric formula of the bismuth calcium titanate-based piezoelectric ceramic material is as follows: caCe (CaCe) x Bi 4-x Ti 4-y (Yb 1/2 Ta 1/2 ) y O 15 +z mol％Nb 2 O 5 Where x=0.06, y=0.02, z=1.
Preparation of bismuth calcium titanate-based piezoelectric ceramic material:
step 1, weighing various raw materials (calcium carbonate CaCO) according to the stoichiometric amount 3 Bismuth oxide Bi 2 O 3 Titanium oxide tTi 2 O 3 CeO of cerium oxide 2 Ytterbium oxide Yb 2 O 3 Tantalum pentoxide Ta 2 O 5 And niobium pentoxide Nb 2 O 5 ) Placing the mixture into a nylon ball milling tank, taking absolute ethyl alcohol as a dispersion medium, mixing and ball milling for 8 hours by using a planetary mill machine with the total mass ratio of the absolute ethyl alcohol to the raw materials being 2:1, drying the slurry at the temperature of 100 ℃ at the rotating speed of 250rpm, presintering at the temperature of 700 ℃, and preserving the heat for 3 hours to obtain presintered powder.
Step 2, performing secondary ball milling on the presintered powder for 24 hours, taking out and drying, adding PVA aqueous solution with the mass fraction of 5wt% as an adhesive, uniformly grinding the PVA aqueous solution with the mass of 12% of the total mass, sieving the PVA aqueous solution with a 60-mesh sieve, and pressing the PVA aqueous solution into a thin round billet with the diameter of 14mm and the thickness of 0.5mm under the pressure of 100 MPa.
And 3, discharging PVA solution from the thin round blank after heat preservation for 1h at 650 ℃, and then sintering the round blank for 3h at 1100 ℃ to obtain the sintered ceramic sheet.
And 4, polishing two sides of the sintered ceramic sheet after sintering, printing a platinum electrode, sintering the electrode at the temperature of 1000 ℃, preserving heat for 20min, and placing the electrode in 220 ℃ silicone oil, applying a direct current electric field of 12kV/mm, and preserving polarization for 20 min.
The piezoelectric properties of the bismuth calcium titanate-based piezoelectric ceramic material obtained in the embodiment are as follows: d, d 33 =20pc/N, dielectric loss tan δ=0.18%, curie temperature T c =780 ℃, 600 ℃ resistivity 2.7X10 6 Ω·cm。
Example 3
The stoichiometric formula of the bismuth calcium titanate-based piezoelectric ceramic material is as follows: caCe (CaCe) x Bi 4-x Ti 4-y (Yb 1/2 Ta 1/2 ) y O 15 +z mol％Nb 2 O 5 Where x=0.1, y=0.03, and z=2.
Preparation of bismuth calcium titanate-based piezoelectric ceramic material:
step 1, weighing various raw materials (calcium carbonate CaCO) according to the stoichiometric amount 3 Bismuth oxide Bi 2 O 3 Titanium oxide Ti 2 O 3 CeO of cerium oxide 2 Ytterbium oxide Yb 2 O 3 Tantalum pentoxide Ta 2 O 5 And niobium pentoxide Nb 2 O 5 ) Placing the mixture into a nylon ball milling tank, taking absolute ethyl alcohol as a dispersion medium, mixing and ball milling for 6 hours by using a planetary mill machine with the total mass ratio of the absolute ethyl alcohol to the raw materials being 2:1, drying the slurry at the temperature of 110 ℃ at the rotating speed of 300rpm, presintering at the temperature of 750 ℃, and preserving the heat for 2 hours to obtain presintered powder.
And 2, performing secondary ball milling on the presintered powder for 18 hours, taking out and drying, adding PVA aqueous solution with the mass fraction of 5wt% as an adhesive, wherein the mass of the PVA aqueous solution is 18% of the total mass, grinding uniformly, sieving by a 60-mesh sieve, and pressing into a thin round billet with the diameter of 14mm and the thickness of 0.5mm by using 100 MPa.
And 3, discharging PVA solution from the thin round blank after heat preservation for 1h at 750 ℃, and then sintering the round blank for 3h at 1110 ℃ to obtain the sintered ceramic sheet.
And 4, polishing two sides of the sintered ceramic sheet after sintering, printing a gold electrode, sintering the electrode at 900 ℃, preserving heat for 20min, and placing the electrode in 230 ℃ silicone oil, applying a direct current electric field of 12kV/mm, and preserving polarization for 20 min.
The piezoelectric properties of the bismuth calcium titanate-based piezoelectric ceramic material obtained in the embodiment are as follows: d, d 33 =19pc/N, dielectric loss tan δ=0.19%, curie temperature T c =780 ℃, 600 ℃ resistivity 3.8x10 6 Ω·cm。
Example 4
The stoichiometric formula of the bismuth calcium titanate-based piezoelectric ceramic material is as follows: caCe (CaCe) x Bi 4-x Ti 4-y (Yb 1/2 Ta 1/2 ) y O 15 +z mol％Nb 2 O 5 Where x=0.02, y=0.05, z=3.
Preparation of bismuth calcium titanate-based piezoelectric ceramic material:
step 1, weighing various raw materials (calcium carbonate CaCO) according to the stoichiometric amount 3 Bismuth oxide Bi 2 O 3 Titanium oxide Ti 2 O 3 CeO of cerium oxide 2 Ytterbium oxide Yb 2 O 3 Tantalum pentoxide Ta 2 O 5 And niobium pentoxide Nb 2 O 5 ) Placing the mixture into a nylon ball milling tank, taking absolute ethyl alcohol as a dispersion medium, mixing and ball milling the mixture for 12 hours by using a planetary mill machine with the rotating speed of 250rpm, drying the slurry at 120 ℃, presintering the slurry at 700 ℃, and preserving the heat for 2 hours to obtain presintered powder.
And 2, performing secondary ball milling on the presintered powder for 18 hours, taking out and drying, adding PVA aqueous solution with the mass fraction of 5wt% as an adhesive, wherein the mass of the PVA aqueous solution is 12% of the total mass, grinding uniformly, sieving by a 60-mesh sieve, and pressing into a thin round billet with the diameter of 14mm and the thickness of 0.5mm by using 100 MPa.
And 3, discharging PVA solution from the thin round blank after heat preservation for 1h at 750 ℃, and then sintering the round blank for 3h at 1080 ℃ to obtain the sintered ceramic sheet.
And 4, polishing two sides of the sintered ceramic sheet after sintering, printing a platinum electrode, sintering the electrode at 800 ℃, preserving heat for 20min, and placing the electrode in 220 ℃ silicone oil, applying a direct current electric field of 15kV/mm, and maintaining for 20min for polarization.
The piezoelectric properties of the bismuth calcium titanate-based piezoelectric ceramic material obtained in the embodiment are as follows: d, d 33 =22pc/N, dielectric loss tan δ=0.27%, curie temperature T c =780 ℃, 600 ℃ resistivity 2.2×10 6 Ω·cm。
Example 5
The stoichiometric formula of the bismuth calcium titanate-based piezoelectric ceramic material is as follows: caCe (CaCe) x Bi 4-x Ti 4-y (Yb 1/2 Ta 1/2 ) y O 15 +z mol％Nb 2 O 5 Where x=0.1, y=0.09, and z=2.
Preparation of bismuth calcium titanate-based piezoelectric ceramic material:
step 1, weighing various raw materials (calcium carbonate CaCO) according to the stoichiometric amount 3 Bismuth oxide Bi 2 O 3 Titanium oxide Ti 2 O 3 CeO of cerium oxide 2 Ytterbium oxide Yb 2 O 3 Tantalum pentoxide Ta 2 O 5 And niobium pentoxide Nb 2 O 5 ) Placing the mixture into a nylon ball milling tank, taking absolute ethyl alcohol as a dispersion medium, mixing and ball milling for 8 hours by using a planetary mill machine with the total mass ratio of the absolute ethyl alcohol to the raw materials being 2:1, drying the slurry at 120 ℃ at the rotating speed of 200rpm, presintering at 750 ℃, and preserving the heat for 2 hours to obtain presintered powder.
And 2, performing secondary ball milling on the presintered powder for 24 hours, taking out and drying, adding PVA aqueous solution with the mass fraction of 5wt% as an adhesive, wherein the mass of the PVA aqueous solution is 12% of the total mass, grinding uniformly, sieving by a 60-mesh sieve, and pressing into a thin round billet with the diameter of 14mm and the thickness of 0.5mm by using 100 MPa.
And 3, discharging PVA solution from the thin round blank after heat preservation for 1h at 850 ℃, and sintering the round blank for 2h at 1050 ℃ to obtain the sintered ceramic sheet.
And 4, polishing two sides of the sintered ceramic sheet after sintering, printing a platinum electrode, sintering the electrode at 800 ℃, preserving heat for 20min, and placing the electrode in 220 ℃ silicone oil, applying a direct current electric field of 12kV/mm, and maintaining for 20min for polarization.
The piezoelectric properties of the bismuth calcium titanate-based piezoelectric ceramic material obtained in the embodiment are as follows: d, d 33 =19pc/N, dielectric loss tan δ=0.18%, curie temperature T c =780 ℃, 600 ℃ resistivity 2.5x10 6 Ω·cm。
Example 6
The stoichiometric formula of the bismuth calcium titanate-based piezoelectric ceramic material is as follows: caCe (CaCe) x Bi 4-x Ti 4-y (Yb 1/2 Ta 1/2 ) y O 15 +z mol％Nb 2 O 5 Where x=0.1, y=0.1, z=4.
Preparation of bismuth calcium titanate-based piezoelectric ceramic material:
step 1, weighing various raw materials (calcium carbonate CaCO) according to the stoichiometric amount 3 Bismuth oxide Bi 2 O 3 Titanium oxide Ti 2 O 3 CeO of cerium oxide 2 Ytterbium oxide Yb 2 O 3 Tantalum pentoxide Ta 2 O 5 And niobium pentoxide Nb 2 O 5 ) Placing the mixture into a nylon ball milling tank, taking absolute ethyl alcohol as a dispersion medium, mixing and ball milling for 8 hours by using a planetary mill machine with the total mass ratio of the absolute ethyl alcohol to the raw materials being 2:1, drying the slurry at 120 ℃ at the rotating speed of 300rpm, presintering at 750 ℃, and preserving the heat for 4 hours to obtain presintered powder.
And 2, performing secondary ball milling on the presintered powder for 12 hours, taking out and drying, adding PVA aqueous solution with the mass fraction of 5wt% as an adhesive, grinding uniformly, sieving with a 60-mesh sieve, and pressing into a thin round blank with the diameter of 14mm and the thickness of 0.5mm under the pressure of 100 MPa.
And 3, discharging PVA solution from the thin round blank after heat preservation for 1h at 600 ℃, and sintering the round blank for 4h at 1180 ℃ to obtain the sintered ceramic sheet.
And 4, polishing two sides of the sintered ceramic sheet after sintering, printing a gold electrode, sintering the electrode at 800 ℃, preserving heat for 20min, and placing the electrode in 220 ℃ silicone oil, applying a direct current electric field of 12kV/mm, and maintaining for 40min for polarization.
The piezoelectric properties of the bismuth calcium titanate-based piezoelectric ceramic material obtained in the embodiment are as follows: d, d 33 =18pc/N, dielectric loss tan δ=0.20%, curie temperature T c =780 ℃, 600 ℃ resistivity 4.8X10 6 Ω·cm。
Table one: performance of each example:
in conclusion, compared with unmodified CaBi 4 Ti 4 O 15 The Curie temperature of the piezoelectric ceramic material of the bismuth calcium titanate base prepared by combining the embodiment 1 of the figure 1 can reach 790 ℃; referring to fig. 2, the depolarization temperature of example 1 reached 600 ℃. The application simultaneously and externally dopes Nb by doping cerium ions at A site, ytterbium ions and tantalum ions at B site of CBT ceramic 2 O 5 Modification is performed so that the bismuth calcium titanate-based piezoelectric ceramic material maintains a high curie temperature (790 ℃) and a piezoelectric constant (from 7.5pC/N to 22 pC/N) and a high temperature resistivity (7×10) 5 The temperature of the mixture is increased to 4.5X10 ℃ at the temperature of Ω cm@600 DEG C 6 The omega cm@600 ℃ is greatly improved, and the material has high-temperature insulativity, so that the material has practical application value in the field of high-temperature piezoelectric sensors.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms should not be understood as necessarily being directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Further, one skilled in the art can engage and combine the different embodiments or examples described in this specification.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (10)
1. A bismuth calcium titanate-based piezoelectric ceramic material is characterized in that cerium ions are doped at A site, ytterbium ions and tantalum ions are doped at B site of CBT ceramic, and Nb is doped at the same time 2 O 5 Modifying;
the stoichiometric amount is CaCe x Bi 4-x Ti 4-y (Yb 1/2 Ta 1/2 ) y O 15 +z mol％Nb 2 O 5 Wherein x is more than 0 and less than or equal to 0.1, y is more than 0 and less than or equal to 0.1, and z is more than 0 and less than or equal to 4.
2. A method for preparing the bismuth calcium titanate-based piezoelectric ceramic material according to claim 1, comprising the steps of:
step 1, weighing various raw materials according to stoichiometric weighing, mixing, ball grinding into slurry, drying the slurry, and presintering to obtain presintered powder;
step 2, after secondary ball milling of the presintered powder, drying, adding an adhesive for grinding and granulating, sieving, and pressing and forming to obtain a thin round blank;
step 3, discharging glue from the thin round blank, and sintering to obtain a sintered ceramic sheet;
and 4, polishing and printing electrodes on two sides of the sintered ceramic sheet, sintering the electrodes, and placing the electrodes in silicone oil to apply voltage for polarization to obtain the bismuth calcium titanate-based piezoelectric ceramic material.
3. The method of claim 2, wherein in step 1, the raw material comprises calcium carbonate CaCO 3 Bismuth oxide Bi 2 O 3 Titanium oxideTi 2 O 3 CeO of cerium oxide 2 Ytterbium oxide Yb 2 O 3 Tantalum pentoxide Ta 2 O 5 And niobium pentoxide Nb 2 O 5 。
4. The preparation method of claim 2, wherein in the step 1, absolute ethyl alcohol is used as a dispersion medium during ball milling, and a planetary mill machine is used for mixed ball milling for 6-12 hours at a rotating speed of 200-300 rpm; during drying, the slurry is dried at the temperature of 100-120 ℃; and (3) presintering at 650-750 ℃ during presintering, and preserving heat for 2-4 hours to obtain presintering powder.
5. The method according to claim 2, wherein in the step 2, the time of the secondary ball milling is 12 to 24 hours.
6. The method according to claim 2, wherein in the step 2, the binder is a polyvinyl alcohol PVA aqueous solution having a mass ratio of 12%.
7. The method according to claim 2, wherein in step 2, the mixture is passed through a 60-mesh sieve and pressed into a thin round billet having a diameter of 12mm to 15mm and a thickness of 0.5mm to 1 mm.
8. The preparation method of claim 2, wherein in the step 3, the PVA solution is discharged after the temperature is kept at 600-850 ℃ for 1 h; sintering is to sinter the thin round billet for 2 to 4 hours at 1050 to 1180 ℃.
9. The method according to claim 2, wherein in step 4, a platinum or gold electrode is printed on the sintered ceramic sheet polished on both sides, and the electrode is sintered at 800 to 1000 ℃ and kept for 10 to 30 minutes.
10. The method according to claim 2, wherein in step 4, a DC electric field of 12kV/mm to 15kV/mm is applied to the silicone oil at 200 ℃ to 240 ℃ for 20min to 40min.
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