CN111725385B - Preparation method of composite PZT piezoelectric film based on sol-gel method and electro-jet deposition method - Google Patents
Preparation method of composite PZT piezoelectric film based on sol-gel method and electro-jet deposition method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000001540 jet deposition Methods 0.000 title claims abstract description 31
- 238000003980 solgel method Methods 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000001035 drying Methods 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 16
- 230000010287 polarization Effects 0.000 claims description 15
- 238000005498 polishing Methods 0.000 claims description 13
- 238000004528 spin coating Methods 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 13
- 238000000137 annealing Methods 0.000 claims description 11
- 238000000151 deposition Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 8
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 8
- 229940046892 lead acetate Drugs 0.000 claims description 8
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims description 8
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 8
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 6
- 239000010936 titanium Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 4
- KQNKJJBFUFKYFX-UHFFFAOYSA-N acetic acid;trihydrate Chemical compound O.O.O.CC(O)=O KQNKJJBFUFKYFX-UHFFFAOYSA-N 0.000 claims description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 230000005684 electric field Effects 0.000 claims description 3
- 230000005484 gravity Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims description 2
- UPRXAOPZPSAYHF-UHFFFAOYSA-N lithium;cyclohexyl(propan-2-yl)azanide Chemical compound CC(C)N([Li])C1CCCCC1 UPRXAOPZPSAYHF-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229940124305 n-propanol Drugs 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000003381 stabilizer Substances 0.000 claims description 2
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical group O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 3
- 230000005621 ferroelectricity Effects 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 72
- 230000003746 surface roughness Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000003292 glue Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 ester compounds Chemical class 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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Abstract
The invention belongs to the technical field of micro electro mechanical systems, and provides a preparation method of a composite PZT piezoelectric film based on a sol-gel method and an electro-jet deposition method. The composite PZT piezoelectric film prepared by the invention has a film thickness of several to hundreds of microns, and compared with a PZT piezoelectric film prepared by a traditional single electric jet deposition method, the composite PZT piezoelectric film has the advantages of reduced micropore defects, improved crystal preferred orientation degree, good combination condition with an upper electrode and a lower electrode, and obviously improved piezoelectric property, ferroelectricity property and other properties.
Description
Technical Field
The invention belongs to the technical field of Micro Electro Mechanical Systems (MEMS), and particularly relates to a method for preparing a PZT piezoelectric thin film by a sol-gel method, a method for preparing a PZT piezoelectric thick film by an electro-jet deposition method and a composite PZT piezoelectric film prepared by combining the advantages of the two methods.
Background
The development of micro-electro-mechanical systems (MEMS) technology has brought tremendous opportunities for the research of microsensors and micro-actuators based on PZT piezoelectric film materials. PZT piezoelectric films are important functional film materials, and due to their excellent ferroelectric, dielectric and piezoelectric properties, they are increasingly paid more attention by researchers in the development and application of MEMS devices.
The Sol-gel method (Sol-gel) is a method of dissolving ester compounds or metal alkoxide in an organic solvent to form a uniform solution, then adding other components, reacting at a certain temperature to form gel, and finally drying to prepare a product, and has the advantages of simple operation, low cost, easy control of stoichiometric ratio, easy doping and the like. The PZT piezoelectric film prepared by the sol-sol method has the advantages of good uniformity, low surface roughness, few defects, excellent microstructure and electrical properties. However, due to the limitation of the method, the thickness of the prepared PZT piezoelectric film is difficult to break through to more than 2 μm, the piezoelectric capability of the piezoelectric film is limited, and the further development of the PZT piezoelectric film in the fields of microsensors, micro actuators and the like is hindered.
The electro-Jet Deposition (electro-hydrodynamic Jet Deposition) is a micro-droplet Jet Deposition molding technology based on electrohydrodynamics, is used as a micro-nano scale additive manufacturing technology, and has the advantages of high molding precision, strong controllability, strong adaptability of a substrate and a Deposition material and the like. The PZT piezoelectric film prepared by the electro-jet deposition method has wide film thickness range, and the film thickness can be from several micrometers to hundreds of micrometers. However, the PZT piezoelectric film prepared by the electro-jet deposition method has the defects of large surface roughness, poor combination condition with an electrode, internal micropore defect and the like.
Therefore, the advantages and the disadvantages of the PZT piezoelectric film prepared by the sol-gel method and the electro-jet deposition method are comprehensively considered, the novel composite PZT piezoelectric film is provided, the film thickness of the PZT piezoelectric film can reach several to hundreds of microns, the film quality and the combination condition of the PZT piezoelectric film and the upper and lower electrodes are improved, and the performance of the film is improved.
Disclosure of Invention
The invention provides a novel composite PZT piezoelectric film aiming at the limitations of film thickness of a PZT piezoelectric film prepared by a sol-gel method and the limitations of large surface roughness, poor combination with an electrode and internal micropore defects of the PZT piezoelectric film prepared by an electro-jet deposition method.
The technical scheme of the invention is as follows:
the preparation method of the composite PZT piezoelectric film based on the sol-gel method and the electro-jet deposition method comprises the following steps:
(1) preparing a bottom PZT piezoelectric film (structure 5 in FIG. 1) with the thickness of 500-800nm by a sol-gel method on a monocrystalline silicon substrate on which an insulating layer and a sputtering bottom electrode are formed;
(2) electro-jet deposition of PZT suspension layer: depositing a layer of PZT suspension by an electro-jet deposition method, wherein the deposition height is 3-5mm, and the deposition flow is 1.5 multiplied by 10-10-2×10-10m3/s；
(3) Drying and pyrolyzing: firstly, drying for 50-70s at the temperature of 150-;
(4) spin coating PZT sol: spin-coating PZT sol on the surface of the material obtained in the step (3), at a low speed of 500-1000r/min for 5-10s, at a high speed of 2500-3500r/min for 25-35s, and spin-coating 2-3 layers;
(5) drying and pyrolyzing: each layer of sol needs to be baked for 4-6min at the temperature of 150-;
(6) then placing the mixture at the temperature of 700-750 ℃ for heat preservation for 10-20 min, and quickly annealing; the thickness of the PZT suspension layer crystallized piezoelectric film deposited by the electric jet after annealing is 800-1200 nm, and the thickness of the spin-coated PZT sol layer crystallized piezoelectric film is 100-200nm (structure 6 and structure 7 in figure 1);
(7) repeating the steps (2) to (6) until the film thickness reaches the thickness of the composite PZT piezoelectric film;
(8) mechanically grinding and polishing the prepared PZT piezoelectric film; then preparing a top-layer PZT piezoelectric film (a structure 10 in a figure 1) with the thickness of 500-800nm by using a sol-gel method; followed by sputtering of the top electrode (fig. 1 structure 11 and structure 12); and finally, carrying out polarization treatment on the whole PZT piezoelectric film.
The monocrystalline silicon substrate (structure 1 in fig. 1) is an n-type (100) single-side polished monocrystalline silicon wafer with the thickness of 200-300 μm.
The insulating layer (figure 1 structure 2) is SiO oxidized by dry oxygen2The thickness is 400-800 nm.
The bottom electrode (structure 3 and structure 4 in FIG. 1) and the top electrode (structure 11 and structure 12 in FIG. 1) are magnetron sputtering Ti (40-60nm)/Pt (150-250nm) metal electrodes.
The thicknesses of the bottom layer PZT piezoelectric film (structure 5 in figure 1) and the top layer PZT piezoelectric film (structure 10 in figure 1) are 500-800 nm.
The suspension used for the electro-jet deposition of the PZT suspension layer (fig. 1, structure 6 and structure 8) is prepared by placing PZT powder in a sol mainly formed by mixing titanium isopropoxide, zirconium n-propoxide, glacial acetic acid, n-propanol and lead acetate trihydrate, wherein the percentage of titanium isopropoxide: zirconium n-propoxide: the mass ratio of the lead acetate trihydrate is 1 (1.4-1.6) to 2.7-2.9); glacial acetic acid: the volume ratio of the n-propanol is 1 (1.3-1.5); the sol-solid-liquid ratio is 0.5-0.6 g/mL; then adding glacial acetic acid, n-propanol and dispersing agent (adding 9-11g of PZT powder, 1-3mL of glacial acetic acid, 2-3mL of n-propanol and 0.1-0.3g of dispersing agent in every 10mL of sol), and carrying out ball milling treatment to obtain the product.
The sol used for spin coating the PZT sol layer (structure 7 and structure 9 in figure 1) is the same as the sol used for preparing the bottom layer and the top layer PZT piezoelectric films, wherein zirconium nitrate, lead acetate and butyl titanate are metal ion sources, ethylene glycol monomethyl ether is a solvent, acetylacetone is a stabilizer (the mass ratio of zirconium nitrate to lead acetate is 1 (1.9-2.1), the volume ratio of butyl titanate to ethylene glycol monomethyl ether to acetylacetone is 1 (15-16) to (1.2-1.3), and the sol-to-liquid ratio is 0.2-0.3g/mL, and the sol is fully mixed and placed to obtain the stable PZT precursor sol.
The mechanical grinding and polishing uses a rotary swinging gravity type grinding and polishing machine, the rotating speed is 60-80rpm, and the polishing time is 20-70 min.
The polarization treatment conditions are that the polarization electric field intensity is 1-2kV/mm, the polarization temperature is 200 ℃ and 300 ℃, and the polarization time is 15-25 min.
The dispersing agent is a titanic acid coupling agent LICA 38.
The invention has the beneficial effects that: the PZT piezoelectric film prepared by the bottom layer sol-gel method ensures that the whole PZT piezoelectric film is well combined with the bottom electrode and guides the epitaxial growth of the PZT piezoelectric film; the PZT piezoelectric film prepared by the electro-jet deposition method ensures the thickness of the whole PZT piezoelectric film; the PZT sol infiltration reduces the micropore defect of the PZT piezoelectric film prepared by the electro-jet deposition method and promotes the preferred orientation of the crystal; the PZT piezoelectric film prepared by mechanical grinding and polishing and a top layer sol-gel method reduces the surface roughness of the whole PZT piezoelectric film and improves the combination condition of the PZT piezoelectric film and a top electrode; after polarization treatment, the PZT piezoelectric film shows excellent piezoelectric performance. The thickness of the composite PZT piezoelectric film prepared by the method can reach several to hundreds of microns, and compared with the PZT piezoelectric film prepared by the traditional single electric jet deposition method, the composite PZT piezoelectric film has the advantages that the defect of microporosities is reduced, the preferred crystal orientation degree is improved, the combination condition with the upper electrode and the lower electrode is good, and the performances such as piezoelectricity, ferroelectricity and the like are obviously improved.
Drawings
FIG. 1 is a schematic cross-sectional view of a composite PZT piezoelectric film prepared according to the present invention based on a sol-gel method and an electro-jet deposition method. In the figure: 1-single crystal Si substrate, 2-SiO2The insulation layer, the bottom PZT piezoelectric film prepared by a 3-Ti, 4-Pt, 5-sol-gel method, the PZT piezoelectric film prepared by a 6, 8-electro-jet deposition method, the 7, 9-spin coating PZT sol layer, the top PZT piezoelectric film prepared by a 10-sol-gel method, and 11-Ti, 12-Pt.
FIG. 2 is a flow chart of a preparation method of the composite PZT piezoelectric film based on a sol-gel method and an electro-jet deposition method.
Detailed Description
The following further describes the specific embodiments of the present invention with reference to the drawings and technical solutions:
as shown in fig. 2, the composite PZT piezoelectric film based on the sol-gel method and the electro-jet deposition method is prepared by the following steps:
preparing a substrate, wherein the substrate is an n-type (100) single-side polished monocrystalline silicon wafer with the thickness of 250 mu m, and the substrate is cleaned for later use. FIG. 1 Structure 1.
Secondly, oxidizing the substrate, and oxidizing SiO with the thickness of 600nm by dry oxygen2An insulating layer. Fig. 1 structure 2.
And step three, sputtering a bottom electrode, and carrying out magnetron sputtering on a Ti (50nm)/Pt (200nm) metal electrode layer. Fig. 1 structure 3 and structure 4.
Step four, preparing a bottom layer PZT by a sol-gel method, preparing PZT sol, spin-coating and spin-drying (low speed 600r/min, spin-drying time 9s, high speed 3000r/min, spin-drying time 30s), drying and pyrolyzing (baking 5min at 180 ℃ and then baking 5min at 350 ℃) and double-layer annealing and crystallizing (heat preservation 8min at 600 ℃ and rapid annealing), and preparing the bottom layer PZT piezoelectric film with the film thickness of 500-800 nm. Fig. 1 structure 5.
Step five, depositing PZT suspension liquid by electric jet flow, preparing the PZT suspension liquid, wherein the deposition height is 4mm, and the deposition flow is 1.67 multiplied by 10-10m3A layer of PZT suspension was deposited and dried for pyrolysis (60 s at 200 ℃ C. and then 60s at 350 ℃ C.).
And sixthly, spin-coating PZT sol, spin-coating 2-3 layers of PZT sol (low speed 600r/min, glue homogenizing time 9s, high speed 3000r/min, glue homogenizing time 30s), and drying and pyrolyzing each layer of PZT sol (hot-drying at 180 ℃ for 5min, and then at 350 ℃ for 5 min).
And seventhly, annealing and crystallizing, keeping the temperature at 720 ℃ for 15min, rapidly annealing, wherein the thickness of the piezoelectric film for crystallizing the PZT suspension layer by the electro-jet deposition after annealing is 800-1200 nm, and the thickness of the piezoelectric film for crystallizing the spin-coated PZT sol layer is 100-200 nm. Fig. 1 structure 6 and structure 7.
And step eight, mechanically grinding and polishing, and if the film thickness does not reach the set thickness, repeating the step five, the step six and the step seven until the film thickness reaches the set thickness. The mechanical grinding and polishing uses a rotary swing gravity type grinding and polishing machine, the rotating speed is 70rpm, and the polishing time is 60 min.
And step nine, preparing the top PZT by a sol-gel method, preparing PZT sol, spin-coating and spin-drying (low speed 600r/min, spin-drying time 9s, high speed 3000r/min, spin-drying time 30s), drying and pyrolyzing (baking for 5min at 180 ℃ and then baking for 5min at 350 ℃) and double-layer annealing and crystallizing (heat preservation for 8min at 600 ℃ and rapid annealing), and preparing the top PZT piezoelectric film with the film thickness of 500-800 nm. Fig. 1 shows a structure 10.
Step ten, sputtering a top electrode, and carrying out magnetron sputtering on a Ti (50nm)/Pt (200nm) metal electrode layer. Fig. 1 structure 11 and structure 12.
And eleventh, carrying out polarization treatment, wherein after the preparation of the integral PZT piezoelectric film is finished, the polarization process operation of the PZT piezoelectric film is carried out under the polarization conditions of the electric field intensity of 1.1kV/mm, the polarization temperature of 250 ℃ and the polarization time of 20 min.
In conclusion, the preparation of the composite PZT piezoelectric film based on the sol-gel method and the electro-jet deposition method is completed. The method integrates the advantages of a gel-sol method and an electro-jet deposition method for preparing the PZT piezoelectric film, the prepared composite PZT piezoelectric film has the film thickness which breaks through the limitation of the sol-gel method and can reach several to hundreds of microns, and the composite PZT piezoelectric film has obvious gain effect compared with the PZT piezoelectric film prepared by the traditional single electro-jet deposition method in the aspects of microstructure, combination conditions of an upper electrode and a lower electrode, piezoelectric ferroelectricity and other properties.
Claims (9)
1. A preparation method of a composite PZT piezoelectric film based on a sol-gel method and an electro-jet deposition method is characterized by comprising the following steps:
(1) preparing a bottom PZT piezoelectric film with the thickness of 500-800nm on a monocrystalline silicon substrate on which an insulating layer and a sputtering bottom electrode are formed by a sol-gel method;
(2) electro-jet deposition of PZT suspension layer: depositing a layer of PZT suspension by an electro-jet deposition method, wherein the deposition height is 3-5mm, and the deposition flow is 1.5 multiplied by 10-10-2×10-10m3/s；
(3) Drying and pyrolyzing: firstly, drying for 50-70s at the temperature of 150-;
(4) spin coating PZT sol: spin-coating PZT sol on the surface of the material obtained in the step (3), at a low speed of 500-1000r/min for 5-10s, at a high speed of 2500-3500r/min for 25-35s, and spin-coating 2-3 layers;
(5) drying and pyrolyzing: each layer of sol needs to be baked for 4-6min at the temperature of 150-;
(6) then placing the mixture at the temperature of 700-750 ℃ for heat preservation for 10-20 min, and quickly annealing; the thickness of the PZT suspending liquid layer crystallized piezoelectric film deposited by the electric jet after annealing is 800-1200 nm, and the thickness of the spin-coated PZT sol layer crystallized piezoelectric film is 100-200 nm;
(7) repeating the steps (2) to (6) until the film thickness reaches the thickness of the composite PZT piezoelectric film;
(8) mechanically grinding and polishing the prepared PZT piezoelectric film; then preparing a top-layer PZT piezoelectric film with the thickness of 500-800nm by using a sol-gel method; then sputtering a top electrode; and finally, carrying out polarization treatment on the whole PZT piezoelectric film.
2. The method as claimed in claim 1, wherein the single crystal silicon substrate is an n-type (100) single-side polished single crystal silicon wafer with a thickness of 200-300 μm.
3. The production method according to claim 1 or 2, wherein the insulating layer is SiO oxidized with dry oxygen2The thickness is 400-800 nm.
4. The method as claimed in claim 3, wherein the bottom electrode and the top electrode are metal electrodes formed by magnetron sputtering of 40-60nm Ti and 150-250nm Pt.
5. The method for preparing according to claim 1, 2 or 4, wherein the suspension used for the electro-jet deposition of the PZT suspension is prepared by placing PZT powder in a sol mainly formed by mixing titanium isopropoxide, zirconium n-propoxide, glacial acetic acid, n-propanol and lead acetate trihydrate, wherein the ratio of titanium isopropoxide: zirconium n-propoxide: the mass ratio of the lead acetate trihydrate is 1 (1.4-1.6) to 2.7-2.9); glacial acetic acid: the volume ratio of the n-propanol is 1 (1.3-1.5); the sol-solid-liquid ratio is 0.5-0.6 g/mL; then adding glacial acetic acid, n-propanol and dispersing agent, adding 9-11g PZT powder, 1-3mL glacial acetic acid, 2-3mL n-propanol and 0.1-0.3g dispersing agent into every 10mL sol, and ball-milling to obtain the final product.
6. The preparation method according to claim 5, wherein the sol used for spin coating the PZT sol layer is the same as the sol used for preparing the bottom and top PZT piezoelectric films, wherein zirconium nitrate, lead acetate and butyl titanate are used as metal ion sources, ethylene glycol monomethyl ether is used as a solvent, and acetylacetone is used as a stabilizer; zirconium nitrate: the mass ratio of the lead acetate is 1 (1.9-2.1); butyl titanate: ethylene glycol methyl ether: the volume ratio of acetylacetone is 1 (15-16) to 1.2-1.3, and the sol-solid-liquid ratio is 0.2-0.3 g/mL; fully mixing, and standing to obtain the stable PZT precursor sol.
7. The method according to claim 1, 2, 4 or 6, wherein the mechanical grinding and polishing is performed by using a rotary oscillating gravity grinding and polishing machine with a rotation speed of 60-80rpm and a polishing time of 20-70 min.
8. The method as claimed in claim 7, wherein the polarization treatment conditions are a polarization electric field strength of 1-2kV/mm, a polarization temperature of 200-.
9. The method according to claim 5, wherein the dispersant is a titanic acid coupling agent LICA 38.
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| JP5471612B2 (en) * | 2009-06-22 | 2014-04-16 | 日立金属株式会社 | Method for manufacturing piezoelectric thin film element and method for manufacturing piezoelectric thin film device |
| CN102060531A (en) * | 2010-11-29 | 2011-05-18 | 南京航空航天大学 | Method for preparing PZT (lead zirconate titanate) piezoelectric ceramic film |
| US20170050888A1 (en) * | 2015-08-19 | 2017-02-23 | Cal Poly Pomona Foundation Inc. | Production of Ceramic Metal Oxide Membranes by Means of Reactive Electrospinning |
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