CN110112285A - A kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode - Google Patents
A kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode Download PDFInfo
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Abstract
A kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode, belongs to thin films of piezoelectric material preparation field.Preparation step includes: 1) in SiO2Pt-Ti/Ti/SiO is prepared in magnetron sputtering on/Si substrate2/ Si hearth electrode material；2) using lead acetate, zirconium nitrate and butyl titanate as raw material, acetylacetone,2,4-pentanedione and formamide are stabilizer, and ethylene glycol monomethyl ether is solvent, and preparing chemical formula is Pb (ZryTi1‑y)O3Lead zirconate titanate precursor solution；3) lead zirconate titanate precursor solution is respectively deposited at Pt-Ti/Ti/SiO2/ Si and Pt/Ti/SiO2It on/Si hearth electrode, and is heat-treated, repeated deposition and heat treatment step obtain the lead zirconate titanate piezoelectric film of (100) preferred orientation afterwards several times.The high lead zirconate titanate piezoelectric film of (100) preferred orientation degree can be made in preparation method of the invention.
Description
Technical field
The invention belongs to thin films of piezoelectric material preparation field, in particular to a kind of high-performance lead zirconate titanate piezoelectric film bottom electricity
The preparation method of pole.
Background technique
Lead zirconate titanate (abbreviation PZT) is to belong to ABO3The perovskite piezoelectric material of type, chemical formula are Pb (ZryTi1-y)O3,
As atomic ratio Zr/Ti=0.52:0.48 or 0.53:0.47, which has good piezoelectricity, dielectric and ferroelectric properties.
In general, the pzt thin film in MEMS as driving unit has generally required preferable piezoelectric property.
Research shows that: the high PZT piezoelectric membrane of (100) preferred orientation degree has higher piezoelectric modulus, is applied on microactrator part
When can be more advantageous.In addition, the base material of pzt thin film has a significant impact to the growth of pzt thin film with performance.Many scholars
By sputtering the more matched buffer layer base material of pzt thin film lattice with (100) preferred orientation, such as SrRuO3、LaNiO3Deng
Prepare the PZT piezoelectric membrane of (100) preferred orientation, but this method price is high and the period is long.The substrate material of another mainstream
Material is exactly Pt/Ti/SiO2/ Si substrate, the wherein effect of metal Ti mainly bonds oxide layer and electrode layer, and Pt and PZT
The lattice constant of film, thermal expansion coefficient more match, and can be used as comparatively ideal hearth electrode material.Meanwhile many research reports
The growth of the diffusion couple pzt thin film of substrate Ti atom has a significant impact.Katsuhiro Aoki et al. pzt thin film and electrode it
Between introduce Ti buffer layer, they have found lead titanates Preferential Nucleation under the action of Ti buffer layer, reduce the crystallization temperature of pzt thin film
Degree, while making the pzt thin film surface grown more uniform, fine and close.
The present invention is in SiO2Ti-Pt/Ti alloy electrode is prepared on/Si substrate, the Ti-Pt for having studied different component is closed
The crystal orientation for the pzt thin film that gold electrode prepares sol-gal process and the influence of electric property.
Summary of the invention
To solve the above problems, the present invention provides a kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode,
The higher lead zirconate titanate piezoelectric film of (100) preferred orientation degree can be made in this method.
The present invention is using lead acetate, zirconium nitrate and butyl titanate as raw material, before preparing lead zirconate titanate using sol-gel method
Liquid solution is driven, and by precursor solution according to being deposited on Pt-Ti/Ti/SiO2On/Si hearth electrode.In Pt-Ti/Ti/SiO2The bottom /Si
In electrode, the Ti layer sputtered in oxide layer mainly plays cementation, and the Ti element deposited simultaneously with Pt then will disperse in Pt layers
Surface deposits (100) preferred orientation degree and electrical property of pzt thin film after being effectively improved.
Technical solution of the present invention:
A kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode, includes the following steps:
1) in SiO2Pt-Ti/Ti/SiO is prepared in magnetron sputtering on/Si substrate2/ Si hearth electrode；
2) using lead acetate, zirconium nitrate and butyl titanate as raw material, acetylacetone,2,4-pentanedione and formamide are stabilizer, ethylene glycol first
Ether is solvent, and adjusts pH by acid-base modifier, and preparing chemical formula is Pb (ZryTi1-y)O3Lead zirconate titanate precursor solution,
Wherein y is 0.51-0.55；
The lead zirconate titanate precursor solution, pH value 3.5-5.6, concentration 0.32-0.52mol/L；
When preparing lead zirconate titanate precursor solution, control lead acetate, zirconium nitrate, butyl titanate, acetylacetone,2,4-pentanedione and formyl
Molar ratio between amine is (1.1-1.3): y:(1-y): (0.80-1.50): (2.00-2.55), wherein for compensation annealing process
A large amount of volatilizations of middle lead element, the accounting range for choosing lead acetate is 1.1-1.3；The proportion of remaining drug is controlled in the range
Within, guarantee to generate the stable and lead zirconate titanate precursor solution without precipitating；The molar ratio for controlling acetylacetone,2,4-pentanedione and formamide, has
Conducive to the quality and stability for improving precursor solution, prevents from generating and precipitate, additionally it is possible to is cracked when film being avoided to deposit.
3) the lead zirconate titanate precursor solution being prepared in step 2) is deposited on Pt-Ti/Ti/SiO2/ Si hearth electrode
It goes up and is heat-treated, lead zirconate titanate piezoelectric film is prepared repeatedly to required thickness in repeated deposition and heat treatment step；Its
Middle heat treatment step includes: first to be dried 5-10 minutes to remove moisture removal at 110-180 DEG C；Then hot at 300-500 DEG C
Decompose 5-10 minutes decomposing organic matters；Finally making annealing treatment at 550-700 DEG C makes film crystallization perovskite knot for 8-15 minutes
Structure, heat treatment process advantageously ensure that the microstructure and dielectric properties of lead zirconate titanate piezoelectric film.
The Pt-Ti/Ti/SiO2The preparation of/Si hearth electrode includes the following steps:
A) control magnetic control sputtering device background vacuum is (3.0-8.0) × 10-5Pa is subsequently charged with pure Ar gas and adjusts and sinks
Pneumatosis pressure is 0.2-1.2Pa, and opening Ti target and corresponding to shielding power supply and regulation power is 0-100W, in SiO2It sinks on/Si substrate
The Ti metal layer of product 30-60nm；
B) under the step a) sedimentary condition, open simultaneously Ti and Pt target and correspond to shielding power supply, adjust metal Ti and
The sputtering power of Pt target is respectively 0-100W and 100-200W, and deposition obtains Pt-Ti/Ti/SiO on Ti metal layer2The bottom /Si
Electrode material；Control Ti and Pt target sputtering power in the range, be conducive to control Pt and Ti deposition rate with
Content facilitates (100) the preferred orientation degree for improving pzt thin film, and then improves the piezoelectric property of film, it is made to be applied to micro- hold
It is more stable when row device.
The preparation of the lead zirconate titanate precursor solution includes the following steps:
C) butyl titanate is added in acetylacetone,2,4-pentanedione solution, obtains mixed liquor A；Mixed liquor A is warming up to 50-60 DEG C,
50-80min is kept the temperature, zirconium nitrate, lead acetate and ethylene glycol monomethyl ether are then sequentially added into mixed liquor A, stirs evenly and is warming up to 70-
100 DEG C, 50-80min is kept the temperature, mixed liquid B is obtained；
D) formamide is added in the mixed liquid B obtained in step c) and stirs evenly, is then cooled to 50-60 DEG C, keeps the temperature 50-
Then acid-base modifier is added into mixed liquid B and keeps the temperature 50-80min, obtains lead zirconate titanate precursor solution by 80min.
The acid-base modifier is acetic acid.
The hearth electrode material surface even compact prepared using the above method, lead zirconate titanate precursor solution are more steady
Fixed, this is all beneficial to the raising of lead zirconate titanate piezoelectric film (100) preferred orientation degree of deposition and the improvement of electrical property.
In the present invention, the lead zirconate titanate precursor solution can be deposited on by hearth electrode using conventional method in that art
On, deposition method for example may include: the lead zirconate titanate precursor solution is spin coating 8-13 seconds lower at 500-700 revs/min,
It is rejection film 30-40 seconds lower at 2600-3000 revs/min again.Aforesaid way can be such that the lead zirconate titanate precursor solution uniformly covers
It covers on the hearth electrode.
Pt-Ti/Ti/SiO prepared by the present invention2/ Si hearth electrode material, can be by normal with thermal oxide etc. on a si substrate
Rule method forms SiO2Layer, then in SiO2Pure ti layers and Pt-Ti alloy-layer are deposited by magnetron sputtering technique on layer, are made
State hearth electrode material.In particular, the hearth electrode is the Pt-Ti/Ti/SiO dried through 110-200 DEG C 8-15 minutes2The bottom /Si electricity
Pole.
The available single layer thickness of preparation method of the invention is the lead zirconate titanate piezoelectric film of 60-85nm；Further,
By repeating the above steps 3), until obtain the multilayer lead zirconate titanate piezoelectric film with target thickness, target thickness for example can be with
It is 1 μm.
The lead zirconate titanate piezoelectric film being prepared by the above method, is applied to microactrator part, and effect is more preferable.
Further, the lead zirconate titanate piezoelectric film of (100) preferred orientation prepared by the present invention shows as pure perovskite knot
Structure；(100) the crystal orientation degree of orientation > 85.7%.
Beneficial effects of the present invention:
1, zirconium-n-propylate is replaced using zirconium nitrate when lead zirconate titanate piezoelectric film prepared by the present invention, reduces and is produced into
This, simplifies operating process.
2, selection Pt-Ti/Ti/SiO of the invention2/ Si hearth electrode material, a large amount of Ti elements are scattered in Pt layer surface, promote
Lead titanates Preferential Nucleation is made, (100) preferred orientation degree and electrical property of pzt thin film is deposited after effectively improving.
When 3, lead zirconate titanate piezoelectric film (100) preferred orientation degree produced by the present invention is up to 85% or more, 0.1kHz
Relative dielectric constant is 1224, and the dielectric properties of dielectric loss 0.056, film are excellent.
Detailed description of the invention
Fig. 1 is the XRD curve of the PZT thin film of section Example of the present invention preparation.
Fig. 2 is the dielectric and magnetic curve of lead zirconate titanate piezoelectric film prepared by embodiment 1.
Fig. 3 is the dielectric and magnetic curve of lead zirconate titanate piezoelectric film prepared by embodiment 2.
Fig. 4 is the dielectric and magnetic curve of lead zirconate titanate piezoelectric film prepared by embodiment 3.
Fig. 5 is the ferroelectric hysteresis loop of the lead zirconate titanate piezoelectric film of section Example of the present invention preparation.
Specific embodiment
Below in conjunction with attached drawing and technical solution, a specific embodiment of the invention is further illustrated.
Embodiment 1
The present embodiment provides in Pt/Ti/SiO2The lead zirconate titanate piezoelectric of (100) preferred orientation deposited on/Si hearth electrode
The preparation method of film, step specifically:
S101, chemical formula is prepared as Pb (ZryTi1-y)O3Lead zirconate titanate precursor solution
For the lead loss in compensation post anneal, lead element excessive 20% is considered when ingredient.First measure 1.7mL levulinic
2.9mL butyl titanate is then dissolved in acetylacetone,2,4-pentanedione and is warming up to 50 DEG C by ketone solution, heat preservation 80 minutes；Then add again
Enter 4.02 grams of zirconium nitrates, 10.53 grams of lead acetates and 26mL ethylene glycol monomethyl ether, be warming up to 70 DEG C after mixing evenly, keeps the temperature 80 minutes；
It is added followed by 1.8mL formamide, stir evenly and is cooled to 50 DEG C, heat preservation 80 minutes；It is eventually adding 12mL acetic acid solution simultaneously
Heat preservation 80 minutes, obtains the lead zirconate titanate precursor solution that pH value is 3.5, concentration is 0.32mol/L.
S102, deposition and heat treatment；
It is Pb (Zr by chemical formulayTi1-y)O3Above-mentioned lead zirconate titanate precursor solution first through 500 revs/min spin coating 13 seconds,
Conventional Pt/Ti/SiO is deposited within spin coating rejection film 40 seconds through 2600 revs/min again2On/Si substrate.After depositing each layer, it will deposit
Wet film at 110 DEG C heat dry and remove moisture removal in 10 minutes, 10 minutes thermal decomposition organic matters are then handled at 300 DEG C, are finally existed
It anneals 8 minutes at 700 DEG C, obtains the lead zirconate titanate piezoelectric film that thickness in monolayer is about 60 rans.
It repeats the above steps to obtaining the lead zirconate titanate piezoelectric film with a thickness of 1 microns.
The XRD spectrum of above-mentioned lead zirconate titanate piezoelectric film and dielectric property at room temperature are shown in Fig. 1 and Fig. 2 respectively.Zirconium metatitanic acid
(100) crystal orientation preferred orientation degree of lead piezoelectric membrane is calculated by formula (1):
In formula (1), α is (100) crystal orientation preferred orientation degree, I(100)、I(110)And I(111)Respectively (100), (110) and
(111) peak intensity of crystal orientation.As seen from Figure 1, above-mentioned lead zirconate titanate piezoelectric film shows as the perovskite knot of (100) preferred orientation
Structure.It is 76.3% by (100) crystal orientation preferred orientation degree that formula (1) calculates.
In addition, the relative dielectric constant of pzt thin film can be calculated by formula (2):
In formula (2), εyFor relative dielectric constant, C is the capacitor that lead zirconate titanate piezoelectric film measures, and d is film thickness, ε0
For permittivity of vacuum, A is the electrode area of film.It is 1032.32 by the relative dielectric constant that formula (2) calculate, dielectric damage
Consumption is 0.044.In addition, as shown in Figure 5, above-mentioned film excess polarization (2Pr) it is 13.38 μ C/cm2, coercive field strength (2Ec) be
51.65kV/cm。
Embodiment 2
The present embodiment provides Pt-Ti/Ti/SiO2The lead zirconate titanate piezoelectric of (100) preferred orientation deposited on/Si hearth electrode
The preparation method of film, step specifically:
S201, preparation Pt-Ti/Ti/SiO2/ Si hearth electrode
The SiO of 100nm thickness is formed by dry oxidation in two inches of Si on pieces2Layer, then the Si piece is put into magnetron sputtering
Deposit metal electrodes on instrument sample stage.Sputter background vacuum is evacuated to 3.0 × 10 before deposition-5Pa is then filled with pure Ar gas
Body simultaneously adjusts deposition pressure as 1Pa, opens Ti target and corresponds to DC power supply and set sputtering power as 80W, opens sample after build-up of luminance
Product baffle, control sedimentation time is 5min, first in SiO2Ti layers of pure metal of 60nm thickness are prepared on/Si substrate.Pure ti layers
Sample baffle is closed after deposition, adjusting sputtering power is 10W, opens simultaneously Pt target and corresponds to DC power supply and set sputtering
Power is 100W, and sample baffle is opened after the normal build-up of luminance of two kinds of targets, and control sedimentation time is 10min, and sputtering obtains Pt-
Ti/Ti/SiO2/ Si hearth electrode material.
S202, chemical formula is prepared as Pb (ZryTi1-y)O3Lead zirconate titanate precursor solution
For the lead loss in compensation post anneal, lead element excessive 20% is considered when ingredient.First measure 1.7mL levulinic
2.9mL butyl titanate is then dissolved in acetylacetone,2,4-pentanedione and is warming up to 60 DEG C by ketone solution, heat preservation 50 minutes；Then add again
Enter 4.02 grams of zirconium nitrates, 10.53 grams of lead acetates and 26mL ethylene glycol monomethyl ether, be warming up to 100 DEG C after mixing evenly, keeps the temperature 50 points
Clock；It is added followed by 1.8mL formamide, stir evenly and is cooled to 60 DEG C, heat preservation 50 minutes；It is eventually adding 12mL acetic acid solution
And 50 minutes are kept the temperature, obtain the lead zirconate titanate precursor solution that pH value is 5.6, concentration is 0.52mol/L.
S203, deposition and heat treatment；
It is Pb (Zr by chemical formulayTi1-y)O3Above-mentioned lead zirconate titanate precursor solution first through 700 revs/min spin coating 8 seconds,
Above-mentioned Pt-Ti/Ti/SiO is deposited within spin coating rejection film 30 seconds through 3000 revs/min again2On/Si hearth electrode.It, will after depositing each layer
The wet film of deposition heat at 200 DEG C, which is dried 8 minutes, removes moisture removal, 5 minutes thermal decomposition organic matters is then handled at 500 DEG C, finally
It anneals 10 minutes at 600 DEG C, obtains the lead zirconate titanate piezoelectric film that thickness in monolayer is about 85 rans.
It repeats the above steps to obtaining the lead zirconate titanate piezoelectric film with a thickness of 1 microns.
The XRD spectrum of above-mentioned lead zirconate titanate piezoelectric film and dielectric property at room temperature are shown in Fig. 1 and Fig. 3 respectively.It can by Fig. 1
Find out, above-mentioned lead zirconate titanate piezoelectric film shows as the pure perovskite knot of height (100) preferred orientation without any Jiao Lvshi phase
Structure.Calculating above-mentioned film (100) crystal orientation preferred orientation degree by formula (1) is 85.7%.When frequency is 0.1kHz, by formula
(2) relative dielectric constant for calculating above-mentioned film is 1224.25, dielectric loss 0.056.In addition, as shown in Figure 5, it is above-mentioned
Film excess polarization (2Pr) up to 20.75 μ C/cm2, and coercive field strength (2Ec) it is only 51.43kV/cm.
Compared with Example 1, lead zirconate titanate piezoelectric film (100) preferred orientation degree produced by the present invention up to 85% with
On, relative dielectric constant reaches 1224.25, dielectric loss 0.056,2PrUp to 20.75 μ C/cm2, and 2EcOnly
The electrical property of 51.43kV/cm, film significantly improve.
Embodiment 3
The present embodiment provides Pt-Ti/Ti/SiO2The lead zirconate titanate piezoelectric of (100) preferred orientation deposited on/Si hearth electrode
The preparation method of film, step specifically:
S301, preparation Pt-Ti/Ti/SiO2/ Si hearth electrode
The SiO of 100nm thickness is formed by dry oxidation in two inches of Si on pieces2Layer, then the Si piece is put into magnetron sputtering
Deposit metal electrodes on instrument sample stage.Sputter background vacuum is evacuated to 5.0 × 10 before deposition-5Pa is then filled with pure Ar gas
Body simultaneously adjusts deposition pressure as 1.2Pa, opens Ti target and corresponds to DC power supply and set sputtering power as 50W, opens after build-up of luminance
Sample baffle, control sedimentation time is 8min, first in SiO2Ti layers of pure metal of 50nm thickness are prepared on/Si substrate.Pure Ti
Sample baffle is closed after layer deposition, adjusting sputtering power is 25W, opens simultaneously Pt target and corresponds to DC power supply and set and splashes
Penetrating power is 150W, and sample baffle is opened after the normal build-up of luminance of two kinds of targets, and control sedimentation time is 8min, and sputtering obtains
Pt-Ti/Ti/SiO2/ Si hearth electrode material.
S302, chemical formula is prepared as Pb (ZryTi1-y)O3Lead zirconate titanate precursor solution
For the lead loss in compensation post anneal, lead element excessive 20% is considered when ingredient.First measure 1.7mL levulinic
2.9mL butyl titanate is then dissolved in acetylacetone,2,4-pentanedione and is warming up to 55 DEG C by ketone solution, heat preservation 65 minutes；Then add again
Enter 4.02 grams of zirconium nitrates, 10.53 grams of lead acetates and 26mL ethylene glycol monomethyl ether, be warming up to 85 DEG C after mixing evenly, keeps the temperature 65 minutes；
It is added followed by 1.8mL formamide, stir evenly and is cooled to 66 DEG C, heat preservation 65 minutes；It is eventually adding 12mL acetic acid solution simultaneously
Heat preservation 65 minutes, obtains the lead zirconate titanate precursor solution that pH value is 4.8, concentration is 0.42mol/L.
S303, deposition and heat treatment；
It is Pb (Zr by chemical formulayTi1-y)O3Above-mentioned lead zirconate titanate precursor solution first through 600 revs/min spin coating 10 seconds,
Above-mentioned Pt-Ti/Ti/SiO is deposited within spin coating rejection film 35 seconds through 2800 revs/min again2On/Si hearth electrode.It, will after depositing each layer
The wet film of deposition heat at 160 DEG C, which is dried 12 minutes, removes moisture removal, 8 minutes thermal decomposition organic matters is then handled at 400 DEG C, finally
It anneals 12 minutes at 650 DEG C, obtains the lead zirconate titanate piezoelectric film that thickness in monolayer is about 75 rans.
It repeats the above steps to obtaining the lead zirconate titanate piezoelectric film with a thickness of 1 microns.
The XRD spectrum of above-mentioned lead zirconate titanate piezoelectric film and dielectric property at room temperature are shown in Fig. 1 and Fig. 4 respectively.It can by Fig. 1
Find out, above-mentioned lead zirconate titanate piezoelectric film still behaves as the pure perovskite structure without any Jiao Lvshi phase.It is in frequency
It is 1191.34 by the relative dielectric constant that formula (2) calculates above-mentioned film when 0.1kHz, dielectric loss 0.059.In addition,
As shown in Figure 5, above-mentioned film excess polarization (2Pr) it is 12.32 μ C/cm2, and coercive field strength (2Ec) it is 57.15kV/cm.
Claims (10)
1. a kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode, which comprises the steps of:
1) in SiO2Pt-Ti/Ti/SiO is prepared in magnetron sputtering on/Si substrate2/ Si hearth electrode；
2) using lead acetate, zirconium nitrate and butyl titanate as raw material, acetylacetone,2,4-pentanedione and formamide are stabilizer, and ethylene glycol monomethyl ether is
Solvent, and pH is adjusted by acid-base modifier, preparing chemical formula is Pb (ZryTi1-y)O3Lead zirconate titanate precursor solution, wherein
Y is 0.51-0.55；
The lead zirconate titanate precursor solution, pH value 3.5-5.6, concentration 0.32-0.52mol/L；
When preparing lead zirconate titanate precursor solution, control lead acetate, zirconium nitrate, butyl titanate, acetylacetone,2,4-pentanedione and formamide it
Between molar ratio be 1.1-1.3:y:1-y:0.80-1.50:2.00-2.55；
3) the lead zirconate titanate precursor solution being prepared in step 2) is deposited on Pt-Ti/Ti/SiO2It goes forward side by side on/Si hearth electrode
Row heat treatment, lead zirconate titanate piezoelectric film is prepared repeatedly to required thickness in repeated deposition and heat treatment step；Wherein at heat
Reason step includes: first to be dried 5-10 minutes to remove moisture at 110-180 DEG C；Then 5-10 is thermally decomposed at 300-500 DEG C
Minute decomposing organic matter；Finally making annealing treatment 8-15 minutes at 550-700 DEG C makes film crystallization perovskite structure.
2. a kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode according to claim 1, feature exist
In the Pt-Ti/Ti/SiO2The preparation of/Si hearth electrode includes the following steps:
A) control magnetic control sputtering device background vacuum is (3.0-8.0) × 10-5Pa is subsequently charged with pure Ar gas and adjusts deposition gas
Pressure is 0.2-1.2Pa, and opening Ti target and corresponding to shielding power supply and regulation power is 0-100W, in SiO230- is deposited on/Si substrate
The Ti metal layer of 60nm；
B) it under the step a) sedimentary condition, opens simultaneously Ti and Pt target and corresponds to shielding power supply, adjust metal Ti and Pt target
The sputtering power of material is respectively 0-100W and 100-200W, and deposition obtains Pt-Ti/Ti/SiO on Ti metal layer2/ Si hearth electrode
Material.
3. a kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode according to claim 1 or 2, feature
It is, the preparation of the lead zirconate titanate precursor solution includes the following steps:
C) butyl titanate is added in acetylacetone,2,4-pentanedione solution, obtains mixed liquor A；Mixed liquor A is warming up to 50-60 DEG C, heat preservation
Then 50-80min sequentially adds zirconium nitrate, lead acetate and ethylene glycol monomethyl ether into mixed liquor A, stir evenly and be warming up to 70-100
DEG C, 50-80min is kept the temperature, mixed liquid B is obtained；
D) formamide is added in the mixed liquid B obtained in step c) and stirs evenly, is then cooled to 50-60 DEG C, keeps the temperature 50-
Then acid-base modifier is added into mixed liquid B and keeps the temperature 50-80min, obtains lead zirconate titanate precursor solution by 80min.
4. a kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode according to claim 1 or 2, feature
It is, the acid-base modifier is acetic acid.
5. a kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode according to claim 3, feature exist
In the acid-base modifier is acetic acid.
6. a kind of according to claim 1, preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode described in 2 or 5, special
Sign is that the deposition method includes the following steps: lead zirconate titanate precursor solution in 500-700 revs/min of lower spin coating 8-
13 seconds, then it is rejection film 30-40 seconds lower at 2600-3000 revs/min.
7. a kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode according to claim 3, feature exist
Include the following steps: in, the deposition method lead zirconate titanate precursor solution is spin coating 8-13 seconds lower at 500-700 revs/min,
It is rejection film 30-40 seconds lower at 2600-3000 revs/min again.
8. a kind of preparation method of high-performance lead zirconate titanate piezoelectric film hearth electrode according to claim 4, feature exist
Include the following steps: in, the deposition method lead zirconate titanate precursor solution is spin coating 8-13 seconds lower at 500-700 revs/min,
It is rejection film 30-40 seconds lower at 2600-3000 revs/min again.
9. according to claim 1, hearth electrode preparation method described in 2,5,7 or 8, which is characterized in that the Pt-Ti/Ti/SiO2/
Si hearth electrode is the hearth electrode dried through 110-200 DEG C 8-15 minutes.
10. the lead zirconate titanate piezoelectric film that preparation method described in -9 is prepared according to claim 1 is applied to microactrator
Part.
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| CN111725385A (en) * | 2020-06-16 | 2020-09-29 | 大连理工大学 | Preparation method of composite PZT piezoelectric film based on sol-gel method and electro-jet deposition method |
| CN114715978A (en) * | 2022-02-21 | 2022-07-08 | 江南大学 | Application of electrochemical cathode of MOS (metal oxide semiconductor) for removing perfluorinated compounds by using hydrated electrons generated by cathode |
| CN114807882A (en) * | 2022-05-06 | 2022-07-29 | 广东省科学院半导体研究所 | Magnetron sputtering target material, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111081864A (en) * | 2020-01-02 | 2020-04-28 | 大连理工大学 | Preparation method of (100) preferred orientation PMN-PZT/PZT heterostructure thin film |
| CN111704162A (en) * | 2020-05-13 | 2020-09-25 | 沈阳工业大学 | Pyrochlore nanocrystalline dielectric film with ultrahigh energy storage performance and preparation thereof |
| CN111704162B (en) * | 2020-05-13 | 2022-05-13 | 沈阳工业大学 | Pyrochlore nanocrystalline dielectric film with ultrahigh energy storage performance and preparation thereof |
| CN111725385A (en) * | 2020-06-16 | 2020-09-29 | 大连理工大学 | Preparation method of composite PZT piezoelectric film based on sol-gel method and electro-jet deposition method |
| CN111725385B (en) * | 2020-06-16 | 2022-04-12 | 大连理工大学 | Preparation method of composite PZT piezoelectric film based on sol-gel method and electro-jet deposition method |
| CN114715978A (en) * | 2022-02-21 | 2022-07-08 | 江南大学 | Application of electrochemical cathode of MOS (metal oxide semiconductor) for removing perfluorinated compounds by using hydrated electrons generated by cathode |
| CN114807882A (en) * | 2022-05-06 | 2022-07-29 | 广东省科学院半导体研究所 | Magnetron sputtering target material, preparation method and application thereof |
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