CN115536392A - Piezoelectric ceramic piece for high-temperature laminated electric driver and preparation method thereof - Google Patents
Piezoelectric ceramic piece for high-temperature laminated electric driver and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 22
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 23
- 229910052573 porcelain Inorganic materials 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- 230000010287 polarization Effects 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 3
- 230000005684 electric field Effects 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 238000006073 displacement reaction Methods 0.000 abstract description 2
- 229910010293 ceramic material Inorganic materials 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
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Abstract
The invention discloses a piezoelectric ceramic piece for a high-temperature laminated piezoelectric driver and a preparation method thereof, belonging to the field of piezoelectric ceramic pieces and preparation methods thereof; the piezoelectric ceramic material provided by the invention has the following chemical formula: pb 0.97 Sr 0.03 (Sb 1/3 Nb 2/3 ) 0.3 (Ni 1/3 Nb 2/3 ) 0.7 O 3 +2wt% Li 2 CO 3 +0.1wt% CuO+0.5wt% Bi 2 O 3 +0.5wt% Li 2 CO 3 (ii) a The preparation method provided by the invention comprises the steps of mixing the raw materials according to the formula, ball milling, drying, presintering, secondary ball milling, drying, press molding, sintering, silver paste printing, silver firing,And (6) polarizing. The piezoelectric ceramic piece provided by the invention has excellent piezoelectric performance, reduces sintering temperature, reduces volatilization of PbO, has larger deformation displacement and better stability, and can meet the use requirement of a high-temperature laminated piezoelectric driver.
Description
Technical Field
The invention relates to a piezoelectric ceramic piece and a preparation method thereof, in particular to a piezoelectric ceramic piece for a high-temperature laminated piezoelectric driver and a preparation method thereof; belongs to the technical field of piezoelectric ceramics.
Background
The low-temperature co-fired laminated piezoelectric driver is formed by alternately stacking ceramic films and electrodes. During the preparation process, because the melting point of the silver element is relatively low, if the sintering temperature is too high, the silver atoms are promoted to diffuse in the ceramic, and the leakage current is increased. Therefore, how to prepare the piezoceramic material for high temperature by the low temperature junction technology is an important research hotspot in the ceramic industry at present.
To date, research on multilayer piezoelectric ceramics prepared by sintering has focused mainly on the composition of PZT-based ceramics, mainly due to their superior piezoelectric properties. Currently, three methods are commonly used to reduce the sintering temperature. Firstly, the sol-gel method is adopted for chemical synthesis, so that the superfine active PZT powder with high surface performance can be obtained, and the driving force for grain growth is increased. Secondly, the holes in the ceramics can be effectively discharged by adopting high-pressure sintering, and the density is improved, thereby reducing the sintering temperature and improving the piezoelectric property. Thirdly, adding a low-temperature sintering aid into the ceramic. Among them, many low melting point glass phases are generated along grain boundaries, promoting grain growth and densifying the ceramic. In addition, the sintering aid replaces Pb in the perovskite solid solution 2+ Or Ti 4+ And structural defects are increased, so that atomic diffusion and electric property improvement are facilitated.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the piezoelectric ceramic sheet for the high-temperature laminated electric driver, which can reduce the sintering temperature and PbO volatilization under the condition of not reducing the piezoelectric performance; another object of the present invention is to provide a method for preparing the piezoelectric ceramic sheet for a high temperature laminated piezoelectric driver.
In order to achieve the purpose, the piezoelectric ceramic piece provided by the invention has the following material composition chemical formula: pb 0.97 Sr 0.03 (Sb 1/3 Nb 2/3 ) 0.3 (Ni 1/3 Nb 2/3 ) 0.7 O 3 +2wt%Li 2 CO 3 +0.1wt%CuO+0.5wt% Bi 2 O 3 +0.5wt% Li 2 CO 3 。
In order to prepare the piezoelectric ceramic sheet for the high-temperature laminated electric driver, the invention adopts the following method:
1) According to the formula Pb 0.97 Sr 0.03 (Sb 1/3 Nb 2/3 ) 0.3 (Ni 1/3 Nb 2/3 ) 0.7 O 3 +2wt%Li 2 CO 3
+0.1wt%CuO+0.5wt% Bi 2 O 3 +0.5wt% Li 2 CO 3 Weighing raw material Pb according to the stoichiometric ratio 3 O 4 、ZrO 2 、TiO 2 、SrCO 3 、Sb 2 O 3 、Nb 2 O 5 、NiO、Li 2 CO 3 、Bi 2 O 3 CuO, li in a mass ratio of 4 2 CO 3 Dividing into A group material and B group material;
2) Raw material Pb 3 O 4 、ZrO 2 、TiO 2 、SrCO 3 、Sb 2 O 3 、Nb 2 O 5 、NiO、Bi 2 O 3 Mixing CuO and the group A material, ball-milling for 4h, and drying to obtain an abrasive;
3) Hermetically calcining the grinding material at 920 ℃ for 2h to obtain a pre-calcined material;
4) Mixing the pre-sintered material with the group B material, performing ball milling for 8 hours, drying, and sieving by a 40-mesh sieve to obtain ceramic powder;
5) Adding polyvinyl alcohol into the porcelain powder, mixing, granulating, and tabletting to obtain a porcelain blank; the addition of polyvinyl alcohol is 5 percent of the weight of the porcelain powder;
6) Sending the porcelain blank into a sintering furnace, heating to 600 ℃, discharging glue for 1h, then heating to 1100-1120 ℃, and sintering for 4h to obtain a porcelain piece;
7) Printing silver paste on the ceramic chip, and then burning silver at 750 ℃ to obtain a silver-coated ceramic chip;
8) And (3) placing the silver ceramic chip in silicone oil at 80 ℃ for polarization for 25min, wherein the electric field polarization strength is 3.5 kv/mm.
Compared with the prior art, the method adopts the technical scheme, and can enable the ceramic to generate liquid phase in the sintering process through the doping of the trace elements, the adjustment of the proportion of lead, zirconium and titanium and the addition of a proper amount of sintering aid, so as to promote the growth of crystal grains (the proper sintering aid can promote the growth of the ceramic crystal grains, and the ceramic sintering is not compact or the electrical property is reduced due to too much or too little sintering aid), therefore, the prepared piezoelectric ceramic piece has excellent piezoelectric property, meanwhile, the sintering temperature is reduced, the volatilization of PbO is reduced, and the piezoelectric ceramic piece has larger deformation displacement and better stability.
The following is the performance comparison data of the piezoelectric ceramic sheet for the high-temperature laminated piezoelectric driver prepared by the method of the invention and the piezoelectric ceramic sheet prepared by the traditional method.
Table 1: comparison table of performance parameters of piezoelectric ceramics prepared by the method and piezoelectric ceramics prepared by the traditional method
The ceramic powder before and after improvement has small performance difference, but the sintering temperature is reduced by nearly 170 ℃, the Curie temperature is reduced by only 3 ℃, and the ceramic powder is very suitable for high-temperature occasions of piezoelectric drivers.
Drawings
FIG. 1 is a micro-morphology diagram of a piezoelectric ceramic chip powder for a high-temperature laminated electric driver provided by the invention;
fig. 2 is an SEM image of a piezoelectric ceramic sheet for a high-temperature laminated electric driver provided by the present invention.
Detailed Description
The invention is further illustrated by the following specific examples:
example 1
1) According to the chemical formula Pb 0.97 Sr 0.03 (Sb 1/3 Nb 2/3 ) 0.3 (Ni 1/3 Nb 2/3 ) 0.7 O 3 +2wt% Li 2 CO 3
+0.1wt% CuO+0.5wt% Bi 2 O 3 +0.5wt% Li 2 CO 3 Weighing raw material Pb according to the stoichiometric ratio 3 O 4 、ZrO 2 、TiO 2 、SrCO 3 、Sb 2 O 3 、Nb 2 O 5 、NiO、Li 2 CO 3 、Bi 2 O 3 CuO, li in a mass ratio of 4 2 CO 3 Dividing into A group material and B group material;
2) Adding Pb 3 O 4 、ZrO 2 、TiO 2 、SrCO 3 、Sb 2 O 3 、Nb 2 O 5 、NiO、Bi 2 O 3 Mixing the CuO and the group A, ball-milling for 4 hours, and drying to obtain an abrasive; the zirconium ball comprises deionized water = 2;
3) Putting the grinding material into a crucible covered and sealed, heating to 920 ℃ at the speed of 2 ℃/min, preserving heat for 2h, and cooling along with a furnace to obtain a pre-sintered material;
4) Mixing the pre-sintered material with the group B material, performing ball milling for 8 hours, drying, and sieving by a 40-mesh sieve to obtain ceramic powder; the mass ratio of the zirconium balls to the deionized water is = 2;
5) Adding polyvinyl alcohol into the porcelain powder, mixing, granulating and pressing into a porcelain blank with the diameter of 10 multiplied by 1 mm; the addition of polyvinyl alcohol is 5 percent of the weight of the porcelain powder;
6) Sending the porcelain blank into a sintering furnace, heating to 600 ℃ at the speed of 1 ℃/min, discharging glue for 1h, then heating to 1100-1120 ℃ at the speed of 2 ℃/min, sintering for 4h, and cooling with the furnace to obtain a porcelain piece;
7) Printing the ceramic chip with the silver paste, then heating to 750 ℃ at the speed of 3 ℃/min, preserving heat for 20min, and cooling along with the furnace to obtain a silver-coated ceramic chip;
8) And (3) placing the silver coated ceramic chip in silicone oil at 80 ℃ for polarization for 25min, wherein the polarization electric field strength is 3.5 kv/mm.
As can be seen from fig. 1-2: the powder after ball milling has uniform particle size, and the consistency of the powder is ensured.
Claims (2)
1. The piezoelectric ceramic sheet for the high-temperature laminated piezoelectric driver is characterized in that the piezoelectric ceramic sheet is made of materials with a chemical formula as follows: pb 0.97 Sr 0.03 (Sb 1/3 Nb 2/3 ) 0.3 (Ni 1/3 Nb 2/3 ) 0.7 O 3 +2wt% Li 2 CO 3 +0.1wt% CuO+0.5wt% Bi 2 O 3 +0.5wt% Li 2 CO 3 。
2. A method for preparing a piezoceramic sheet for a high temperature laminated electric driver according to claim 1, characterized by the steps of:
1) According to the chemical formula Pb 0.97 Sr 0.03 (Sb 1/3 Nb 2/3 ) 0.3 (Ni 1/3 Nb 2/3 ) 0.7 O 3 +2wt% Li 2 CO 3 +0.1wt% CuO+0.5wt% Bi 2 O 3 +0.5wt% Li 2 CO 3 Weighing raw material Pb according to the stoichiometric ratio 3 O 4 、ZrO 2 、TiO 2 、SrCO 3 、Sb 2 O 3 、Nb 2 O 5 、NiO、Li 2 CO 3 、Bi 2 O 3 CuO, li in a mass ratio of 4 2 CO 3 Dividing into A group material and B group material;
2) The raw material Pb is mixed 3 O 4 、ZrO 2 、TiO 2 、SrCO 3 、Sb 2 O 3 、Nb 2 O 5 、NiO、Bi 2 O 3 Mixing CuO and the group A material, ball-milling for 4h, and drying to obtain an abrasive;
3) Hermetically calcining the grinding material at 920 ℃ for 2h to obtain a pre-calcined material;
4) Mixing the pre-sintered material with the group B material, ball-milling for 8 hours, drying, and sieving by a 40-mesh sieve to obtain ceramic powder;
5) Adding polyvinyl alcohol into the porcelain powder, mixing, granulating, and tabletting to obtain a porcelain blank; the addition of the polyvinyl alcohol is 5 percent of the weight of the porcelain powder;
6) Sending the porcelain blank into a sintering furnace, heating to 600 ℃, discharging glue for 1h, then heating to 1100-1120 ℃, and sintering for 4h to obtain a porcelain piece;
7) Printing silver paste on the ceramic chip, and then burning silver at 750 ℃ to obtain a silver-coated ceramic chip;
8) And (3) placing the silver ceramic chip in silicone oil at 80 ℃ for polarization for 25min, wherein the electric field polarization strength is 3.5 kv/mm.
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