CN102584226A - Barium-calcium-zirconium-titanium leadless piezoelectric textured thick film and preparation method of thick film - Google Patents
Barium-calcium-zirconium-titanium leadless piezoelectric textured thick film and preparation method of thick film Download PDFInfo
- Publication number
- CN102584226A CN102584226A CN2012100021973A CN201210002197A CN102584226A CN 102584226 A CN102584226 A CN 102584226A CN 2012100021973 A CN2012100021973 A CN 2012100021973A CN 201210002197 A CN201210002197 A CN 201210002197A CN 102584226 A CN102584226 A CN 102584226A
- Authority
- CN
- China
- Prior art keywords
- thick film
- preparation
- leadless piezoelectric
- template
- barium calcium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention belongs to the field of leadless piezoelectric materials and relates to a leadless piezoelectric textured thick film and a preparation method of the thick film. The chemical components of the leadless piezoelectric textured thick film comply with a chemical formula of (BaxCay)(ZrzTim)O3; and in the chemical formula, x is not less than 0.79 and not more than 0.865, y is not less than 0.135 and not more than 0.21, z is not less than 0.06 and not more than 0.11, and m is not less than 0.89 and not more than 0.94. The preparation method of the thick film comprises the following steps of: (1) preparing corresponding basis material and template; and (2) placing the template and the basis material into a mortar according to a certain proportion, adding a solvent and a bonder, and grinding to prepare a slurry; screen-printing the slurry to obtain a film sheet; carrying out isostatic pressing on the obtained film sheet; and taking out a pressed sample, and carrying out heat treatment on the pressed sample to obtain the leadless piezoelectric textured thick film with good orientation. The leadless piezoelectric textured thick film prepared by the preparation method has higher orientation degree, can be widely applied to the aspects of a piezoelectric sensor, a piezoelectric motor and a high-precision displacement controller and the like, and is beneficial to the development of device miniaturization.
Description
Technical field
The invention belongs to the leadless piezoelectric material material field, be specifically related to the textured method of a kind of leadless piezoelectric structured thick film and leadless piezoelectric structured thick film.
Background technology
Piezoelectric is widely used in present Electronics Science and Technology, comprises the gordian technique in the spationautics, medical science and industrial stopper, transverter, transmitter etc.Widespread use at present be the basic piezoelectric of Pb-based lanthanumdoped zirconate titanates (PZT) of the perovskite typed of lead base; As everyone knows; Preparation, use and discarded last handling process in the lead base material can cause serious harm to the mankind and environment, therefore research and develop environmentally friendly leadless piezoelectric material material and be one urgent and the task of important realistic meaning arranged.
The leadless piezoelectric system of report mainly contains four kinds at present: BaTiO
3Base leadless piezoelectricity material, (Bi
0.5Na
0.5) TiO
3Base leadless piezoelectricity material, niobate lead-free piezoelectric and bismuth laminated leadless piezoelectric.Although bismuth layer structured and bismuth sodium titanate based piezoelectric Tc is high, all more than 600 ℃, its piezoelectric property is relatively poor mostly, the d of bismuth-sodium titanate pottery
3360pC/N is only arranged, and bismuth titanate ceramics has only 20pC/N.The potassium-sodium niobate material density is low, is difficult to sintering.Barium-titanate material research is ripe, and it is superior that sintering, and its piezoelectric property easily compares.Recently, Ren et al finds (Ba
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3Ceramic systems (untextured thick film systems) shows surprising piezoelectric property, and its piezo-electric modulus can reach 620pC/N, and this performance can compare favourably with the lead base material.Subsequently, people such as Liwei improve performance through ion doping, have obtained more superior performance.But present leadless piezoelectric material material mainly is through mixing and the compound performance of improving material.Recent years, many scholars changed performance through the structure of control material, and wherein maximum is exactly the texturing of piezoelectric.The texturing degree of leadless piezoelectric material material can be passed through Lotgering ' s factor (F.K.Lotgering.Topotactical Reactions with Ferrimagnetic Oxides having Hexagonal Crystal Structures-I.Journal of Inorganic and Nuclear Chemistry; 9 (2) (1959), 113-123) characterize.Thick film has many advantages of block and thin-film material concurrently.On the one hand, its thickness block of comparing reduces greatly, thereby has reduced the driving voltage in circuit, can make it be operated in the low voltage high frequency, in unicircuit, using the condition that provides; On the other hand, have the electric property and the anti-fatigue performance that can compare favourably with block materials.Therefore, thick-film material and thick film device receive Materials science worker's concern always.At present, thick-film materials such as more PZT of research and BST have been widely used in various piezoelectricity, ferroelectric, pyroelectric electric device, microwave device and microelectronic mechanical system in radio frequency etc.Than pottery, thick film more helps miniaturization of devices in addition.Yet the textured research of piezoelectric mainly concentrates on the block materials, and thick film mainly is to concentrate on the PZT sill, and the research of lead-free piezoelectric thick film is less, and for (Ba, Ca) (Zr, Ti) O
3The texture lead-free piezoelectric thick film is not then seen report.
Summary of the invention
The object of the present invention is to provide a kind of barium calcium zirconium titanium leadless piezoelectric structured thick film and the textured method of leadless piezoelectric structured thick film.The textured method of leadless piezoelectric structured thick film of the present invention, simple possible can be prepared a kind of high epitaxial leadless piezoelectric structured thick film.
Barium calcium zirconium titanium leadless piezoelectric structured thick film of the present invention, its Chemical Composition meets chemical general formula: (Ba
xCa
y) (Zr
zTi
m) O
3, wherein, 0.79≤x≤0.865,0.135≤y≤021,0.06≤z≤0.11,0.89≤m≤0.94.The mol ratio of each corresponding element represented in the numeral in the element lower right corner or letter in the above-mentioned chemical general formula.
Barium calcium zirconium titanium leadless piezoelectric (Ba of the present invention
xCa
y) (Zr
zTi
m) O
3The preparation method of structured thick film mainly may further comprise the steps:
1) preparation base-material: preparation (Ba
xCa
y) (Zr
zTi
m) O
3(BCZT) matrix of powder material (Ba
aCa
b) (Zr
cTi
d) O
3, wherein, 0.748≤a≤0.8425,0.1575≤b≤0.252,0.072≤c≤0.132,0.87≤d≤0.928.
2) preparation template: adopt BaTiO
3(BT) flaky powder is a template.
3) template that obtains and base-material are prepared burden according to a certain percentage and place mortar, add solvent, ground 3-5 hour, add sticker continuation grinding 0.5-1.5 hour again, make slurry.
4) take out the slurry make, use and draw together template and on platinum, carry out silk screen printing, obtain the diaphragm after the silk screen printing, the diaphragm after the silk screen printing is kept flat leave standstill oven dry, repeat silk screen printing and baking step 2-6 time again; Wait static pressure to handle on the diaphragm after the oven dry, obtain green compact; The green compact that taking-up presses are heat-treated and are obtained the good barium calcium zirconium titanium leadless piezoelectric structured thick film of orientation.
The barium calcium zirconium titanium leadless piezoelectric structured thick film thickness that the present invention obtains is 20-30 μ m.
In the step 1), said BCZT base-material adopts solid reaction process to make, and promptly adopts BaCO
3, CaCO
3, ZrO
2And TiO
2Be raw material, take by weighing BaCO according to the stoichiometric ratio of Ba, Ca, Zr and Ti element in the BCZT base-material
3, CaCO
3, ZrO
2And TiO
2, prepare through batching, batch mixing, precompressed and heat treatment step successively.
In the step 3), template and base-material are prepared burden according to a certain percentage and are meant that the gross weight with template and base-material is the basis, and said template accounts for the 5%-30% of gross weight, and optimal selection is 20%.
Above-mentioned solvent is an absolute ethyl alcohol; Preferably, the add-on of said solvent is the corresponding 25-40ml of adding of the gross weight anhydrous ethanol solvent of 10g template and base-material; The best milling time that the adding solvent grinds is 3 hours.
Above-mentioned sticker is the mixing solutions of Terpineol 350 and TKK 021, and the weight ratio of Terpineol 350 and TKK 021 is 10: (1-1.5).
The viscosity of above-mentioned slurry is dipped into slurry through the amount control of the sticker that adds with glass stick, mentions disposed slurry and can connect into line then viscosity is suitable.
The meshcount of above-mentioned silk screen printing is the 100-300 order, is preferably 200 orders.
The number of times of above-mentioned silk screen printing is 2-6 time, is preferably 3 times; Diaphragm after silk screen printing oven dry each time the time was employed in the baking oven under 110 ℃ constant temperature drying 30 minutes.
When waiting static pressure after the film oven dry of above-mentioned silk screen printing, waiting the pressure of static pressure is 100-250MPa, is preferably 200MPa; Dwell time is 5-15 minute, is preferably 10 minutes.
Above-mentioned heat treated temperature is 1200-1400 ℃, and soaking time is 4-10 hour, and the heat-up rate during thermal treatment is 1-3 ℃/minute.Optimal selection is 1300 ℃ and is incubated 6 hours down.Heat-treat condition can produce certain influence to orientation degree.Preferably in silicon carbide rod furnace, carry out during thermal treatment.
The present invention adopts barium titanate template and (Ba
xCa
y) (Zr
zTi
m) O
3Base-material utilizes screen printing technique successfully to prepare textured (Ba
xCa
y) (Zr
zTi
m) O
3Lead-free piezoelectric thick film.The present invention compared with prior art has following advantage:
1, screen printing technique is the technology of ripe widespread use in the ceramic industry, and preparation cost is low, technology is simple, be fit to large batch of suitability for industrialized production.
2, compare textured (Ba with common prior art
xCa
y) (Zr
zTi
m) O
3Lead-free piezoelectric thick film shows excellent orientation, and the texture degree can reach 81%, has overcome the low difficult problem of orientation degree in the ordinary skill.
3, textured (Ba
xCa
y) (Zr
zTi
m) O
3Lead-free piezoelectric thick film does not almost change the Tc of material.
4, (Ba of the present invention
xCa
y) (Zr
zTi
m) O
3Leadless piezoelectric structured thick film is for the development of miniaturization of devices, chip type lays the first stone.
The orientation degree of the leadless piezoelectric structured thick film that preparation method of the present invention obtains is higher, can be widely used in aspects such as piezoelectric transducer, piezoelectric motors and high precision position shift controller, helps the development of miniaturization of devices.
Description of drawings
Fig. 1 is that template content is 5% textured (Ba among the embodiment 1
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3The X ray diffracting spectrum of lead-free piezoelectric thick film.
Template content is 20% textured (Ba among Fig. 2 embodiment 2
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3The X ray diffracting spectrum of lead-free piezoelectric thick film.
Template content is 30% textured (Ba among Fig. 3 embodiment 3
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3The X ray diffracting spectrum of lead-free piezoelectric thick film.
Template content is 20% textured (Ba among Fig. 4 embodiment 2
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3The SEM figure of lead-free piezoelectric thick film.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment only are used to the present invention is described and are not used in restriction protection scope of the present invention.
Embodiment 1:
(Ba
0.8425Ca
0.1575) (Zr
0.105Ti
0.895) O
3The preparation of base-material: adopt BaCO
3, CaCO
3, ZrO
2And TiO
2Be raw material, according to (Ba
0.8425Ca
0.1575) (Zr
0.105Ti
0.895) O
3The stoichiometric ratio of Ba, Ca, Zr and Ti element adopts solid reaction process to make in the base-material.During preparation, raw mix prepares through precompressed and heat treatment step successively, and wherein the processing condition of precompressed are 2MPa constant voltage 1 minute, and heat treated temperature is 1300 ℃, and the time is 4 hours.
Take by weighing 0.5g barium titanate template and 9.5g (Ba
0.8425Ca
0.1575) (Zr
0.105Ti
0.895) O
3Base-material places mortar, adds absolute ethyl alcohol 25ml and grinds 3 hours, adds the sticker for preparing and continues to grind 1 hour, and said sticker is the mixing solutions of Terpineol 350 and TKK 021, and its both weight ratio is 10: 1.Take out the slurry of preparation, choose 200 purpose plates for screen printing, on the platinum sheet, carry out silk screen printing, every brush one deck was dried 30 minutes in 110 ℃ baking oven, repeatedly triplicate.Stick the intact film of silk screen printing with aluminum oxide and to wait static pressure together, pressure is 200MPa, and waiting the static pressure time is 10 minutes.Taking-up waits the good sample of static pressure, in silicon carbide rod furnace, heat-treats, and thermal treatment temp is 1300 ℃ of insulations 6 hours, and temperature rise rate is 2 ℃/minute, prepares the good (Ba of orientation degree
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3Lead-free piezoelectric thick film.The thickness of this leadless piezoelectric structured thick film is 21 μ m.
Fig. 1 is (Ba
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3The X ray diffracting spectrum of lead-free piezoelectric thick film can find out to have only the uhligite phase structure on scheming, do not observe other dephasigns.Through X ray diffracting spectrum, calculate (Ba
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3Lotgering ' the s factor F=46% of lead-free piezoelectric thick film.
Embodiment 2:
(Ba
0.82Ca
0.18) (Zr
0.12Ti
0.88) O
3The preparation of base-material: adopt BaCO
3, CaCO
3, ZrO
2And TiO
2Be raw material, according to (Ba
0.82Ca
0.18) (Zr
0.12Ti
0.88) O
3The stoichiometric ratio of Ba, Ca, Zr and Ti element adopts solid reaction process to make in the base-material.During preparation, raw mix prepares through precompressed and heat treatment step successively, and wherein the processing condition of precompressed are 2MPa constant voltage 1 minute, and heat treated temperature is 1300 ℃, and the time is 4 hours.
Take by weighing 2g barium titanate template and 8g (Ba
0.82Ca
0.18) (Zr
0.12Ti
0.88) O
3Base-material places mortar, adds absolute ethyl alcohol 25ml and grinds 3 hours, adds the sticker for preparing and continues to grind 1 hour, and said sticker is the mixing solutions of Terpineol 350 and TKK 021, and its both weight ratio is 10: 1.2.Take out the slurry of preparation, choose 200 purpose plates for screen printing, on the platinum sheet, carry out silk screen printing, every brush one deck was dried 30 minutes in 110 ℃ baking oven, repeatedly triplicate.Stick the intact film of silk screen printing with aluminum oxide and to wait static pressure together, pressure is 200MPa, and waiting the static pressure time is 10 minutes.Taking-up waits the good sample of static pressure, in silicon carbide rod furnace, heat-treats, and thermal treatment temp is 1300 ℃ of insulations 6 hours, and temperature rise rate is 2 ℃/minute, prepares the good (Ba of orientation degree
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3Lead-free piezoelectric thick film.The thickness of this leadless piezoelectric structured thick film is 22 μ m.
Fig. 2 is (Ba
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3The X ray diffracting spectrum of lead-free piezoelectric thick film can find out to have only the uhligite phase structure on scheming, do not observe other dephasigns.Through X ray diffracting spectrum, Lotgering ' the s factorF=81% that calculates has obtained the good (Ba of orientation degree
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3Lead-free piezoelectric thick film.Fig. 4 is the textured (Ba that present embodiment obtains
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3Lead-free piezoelectric thick film SEM figure, can know that prepared leadless piezoelectric structured thick film is dense, and density is relatively good.
Embodiment 3:
(Ba
0.805Ca
0.195) (Zr
0.13Ti
0.87) O
3The preparation of base-material: adopt BaCO
3, CaCO
3, ZrO
2And TiO
2Be raw material, according to (Ba
0.805Ca
0.195) (Zr
0.13Ti
0.87) O
3The stoichiometric ratio of Ba, Ca, Zr and Ti element adopts solid reaction process to make in the base-material.During preparation, raw mix prepares through precompressed and heat treatment step successively, and wherein the processing condition of precompressed are 2MPa constant voltage 1 minute, and heat treated temperature is 1300 ℃, and the time is 4 hours.
Take by weighing 3g barium titanate template and 7g (Ba
0.805Ca
0.195) (Zr
0.13Ti
0.87) O
3Base-material places mortar, adds absolute ethyl alcohol 25ml and grinds 3 hours, adds the sticker for preparing and continues to grind 1 hour, and said sticker is the mixing solutions of Terpineol 350 and TKK 021, and its both weight ratio is 10: 1.5.Take out the slurry of preparation, choose 200 purpose plates for screen printing, on the platinum sheet, carry out silk screen printing, every brush one deck was dried 30 minutes in 110 ℃ baking oven, repeatedly triplicate.Stick the intact film of silk screen printing with aluminum oxide and to wait static pressure together, pressure is 200MPa, and waiting the static pressure time is 10 minutes.Taking-up waits the good sample of static pressure, in silicon carbide rod furnace, heat-treats, and thermal treatment temp is 1300 ℃ of insulations 6 hours, and temperature rise rate is 2 ℃/minute, prepares the good (Ba of orientation degree
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3Lead-free piezoelectric thick film.The thickness of this leadless piezoelectric structured thick film is 24 μ m.
Fig. 3 is (Ba
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3The X ray diffracting spectrum of lead-free piezoelectric thick film can find out to have only the uhligite phase structure on scheming, do not observe other dephasigns.Through X ray diffracting spectrum, calculate (Ba
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3Lotgering ' the s factor F=72% of lead-free piezoelectric thick film has obtained the good (Ba of orientation degree
0.85Ca
0.15) (Zr
0.1Ti
0.9) O
3Lead-free piezoelectric thick film.
Embodiment 4
Method preparation (Ba according to embodiment 2
0.748Ca
0.252) (Zr
0.132Ti
0.868) O
3Base-material.Take by weighing 2g barium titanate template and 8g (Ba
0.748Ca
0.252) (Zr
0.132Ti
0.868) O
3Base-material places mortar, adds absolute ethyl alcohol 25ml and grinds 5 hours, adds the sticker (Terpineol 350 and TKK 021 mixing solutions) for preparing and continues to grind 1.5 hours.Take out the slurry of preparation, choose 250 purpose plates for screen printing, on the platinum sheet, carry out silk screen printing, every brush one deck was dried 30 minutes in 110 ℃ baking oven, repeatedly triplicate.Stick the intact film of silk screen printing and aluminum oxide that to wait static pressure, pressure be 100MPa together.Taking-up waits the good sample of static pressure, in silicon carbide rod furnace, heat-treats, and thermal treatment temp is 1200 ℃ of insulations 10 hours, and temperature rise rate is 1 ℃/minute, prepares the good (Ba of orientation degree
0.79Ca
0.21) (Zr
0.11Ti
0.89) O
3Lead-free piezoelectric thick film.The thickness of this leadless piezoelectric structured thick film is 25 μ m.
Through detecting (the Ba that present embodiment obtains
0.79Ca
0.21) (Zr
0.11Ti
0.89) O
3The X ray diffracting spectrum of leadless piezoelectric structured thick film can find out to have only the uhligite phase structure, does not observe other dephasigns.Through X ray diffracting spectrum, Lotgering ' the s factor F=76% that calculates has obtained the good (Ba of orientation degree
0.79Ca
0.21) (Zr
0.11Ti
0.89) O
3Lead-free piezoelectric thick film.
Embodiment 5
Method preparation (Ba according to embodiment 2
0.838Ca
0.162) (Zr
0.072Ti
0.928) O
3Base-material.Take by weighing 2g barium titanate template and 8g (Ba
0.838Ca
0.162) (Zr
0.072Ti
0.928) O
3Base-material places mortar, adds absolute ethyl alcohol 30ml and grinds 3 hours, adds the sticker (Terpineol 350 and TKK 021 mixing solutions) for preparing and continues to grind 1 hour.Take out the slurry of preparation, choose 150 purpose plates for screen printing, on the platinum sheet, carry out silk screen printing, every brush one deck was dried 30 minutes in 110 ℃ baking oven, repeated repeatedly four times.Stick the intact film of silk screen printing and aluminum oxide that to wait static pressure, pressure be 250MPa together.Taking-up waits the good sample of static pressure, in silicon carbide rod furnace, heat-treats, and thermal treatment temp is 1400 ℃ of insulations 4 hours, and temperature rise rate is 3 ℃/minute, prepares the good (Ba of orientation degree
0.865Ca
0.135) (Zr
0.06Ti
0.94) O
3Lead-free piezoelectric thick film.The thickness of this leadless piezoelectric structured thick film is 30 μ m.
Through detecting (the Ba that present embodiment obtains
0.865Ca
0.135) (Zr
0.06Ti
0.94) O
3The X ray diffracting spectrum of leadless piezoelectric structured thick film can find out to have only the uhligite phase structure, does not observe other dephasigns.Through X ray diffracting spectrum, Lotgering ' the s factor F=78% that calculates has obtained the good (Ba of orientation degree
0.865Ca
0.135) (Zr
0.06Ti
0.94) O
3Lead-free piezoelectric thick film.
Claims (10)
1. barium calcium zirconium titanium leadless piezoelectric structured thick film, its Chemical Composition meets chemical general formula: (Ba
xCa
y) (Zr
zTi
m) O
3, wherein, 0.79≤x≤0.865,0.135≤y≤0.21,0.06≤z≤0.11,0.89≤m≤0.94.
2. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 1 mainly may further comprise the steps:
1) preparation base-material: preparation (Ba
xCa
y) (Zr
zTi
m) O
3Matrix of powder material (Ba
aCa
b) (Zr
cTi
d) O
3, wherein, 0.748≤a≤0.8425,0.1575≤b≤0.252,0.072≤c≤0.132,0.87≤d≤0.928;
2) preparation template: adopt BaTiO
3Flaky powder is a template;
3) template that obtains and base-material are prepared burden according to a certain percentage and place mortar, add solvent, ground 3-5 hour, add sticker continuation grinding 0.5-1.5 hour again, make slurry;
4) take out the slurry that makes, use and draw together template; On platinum, carry out silk screen printing, obtain the diaphragm after the silk screen printing, the diaphragm after the silk screen printing is kept flat leave standstill oven dry, repeat silk screen printing and baking step 2-6 time again; Wait static pressure to handle on the diaphragm after the oven dry, obtain green compact; The green compact that taking-up presses are heat-treated and are obtained said barium calcium zirconium titanium leadless piezoelectric structured thick film.
3. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 2 is characterized in that in the step 3), said solvent is an absolute ethyl alcohol; The add-on of said solvent is the corresponding 25-40ml of adding of the gross weight absolute ethyl alcohol of 10g template and base-material.
4. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 2; It is characterized in that; In the step 3), said sticker is the mixing solutions of Terpineol 350 and TKK 021, and the weight ratio of Terpineol 350 and TKK 021 is 10: (1-1.5).
5. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 2 is characterized in that, in the step 3), template and base-material are prepared burden according to a certain percentage and be meant that the gross weight with template and base-material is the basis, and said template accounts for the 5%-30% of gross weight.
6. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 2 is characterized in that in the step 4), the meshcount of said silk screen printing is the 100-300 order; Thick film after the silk screen printing was 110 ℃ of following constant temperature 30 minutes.
7. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 2 is characterized in that, in the step 4), the pressure of said static pressure such as grade is 100-250MPa; The dwell time of said static pressure such as grade is 5-15 minute.
8. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 2 is characterized in that in the step 4), said heat treated temperature is 1200-1400 ℃, and soaking time is 4-10 hour, and the heat-up rate during thermal treatment is 1-3 ℃/minute; In silicon carbide rod furnace, carry out during said thermal treatment.
9. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 2 is characterized in that, the barium calcium zirconium titanium leadless piezoelectric structured thick film thickness that is obtained is 20-30 μ m.
10. the application of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 1 in piezoelectric transducer, piezoelectric motors and high precision position shift controller.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210002197.3A CN102584226B (en) | 2012-01-05 | 2012-01-05 | Barium-calcium-zirconium-titanium leadless piezoelectric textured thick film and preparation method of thick film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210002197.3A CN102584226B (en) | 2012-01-05 | 2012-01-05 | Barium-calcium-zirconium-titanium leadless piezoelectric textured thick film and preparation method of thick film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102584226A true CN102584226A (en) | 2012-07-18 |
| CN102584226B CN102584226B (en) | 2014-06-25 |
Family
ID=46473566
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210002197.3A Expired - Fee Related CN102584226B (en) | 2012-01-05 | 2012-01-05 | Barium-calcium-zirconium-titanium leadless piezoelectric textured thick film and preparation method of thick film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102584226B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103541014A (en) * | 2013-10-14 | 2014-01-29 | 中国科学院上海硅酸盐研究所 | Lead-free high-voltage active crystal material and preparation method thereof |
| CN105418067A (en) * | 2015-12-08 | 2016-03-23 | 天津大学 | Preparation method of barium calcium zirconate titanate lead-free piezoelectric textured ceramic |
| CN106518053A (en) * | 2015-09-10 | 2017-03-22 | 韩国机械研究院 | Crystal orientation template for BaTiO3-based lead-free piezoelectric ceramics and method for fabricating the same |
| CN107459346A (en) * | 2017-08-11 | 2017-12-12 | 哈尔滨工业大学 | Leadless piezoelectric barium phthalate base textured ceramic of high electric property and its preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486570A (en) * | 2009-02-25 | 2009-07-22 | 同济大学 | Leadless piezoelectric structured thick film and preparation thereof |
| CN102285797A (en) * | 2011-06-09 | 2011-12-21 | 同济大学 | Preparation method of KNN (K0.5Na0.5NbO3)-based piezoelectric texture thick film |
-
2012
- 2012-01-05 CN CN201210002197.3A patent/CN102584226B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486570A (en) * | 2009-02-25 | 2009-07-22 | 同济大学 | Leadless piezoelectric structured thick film and preparation thereof |
| CN102285797A (en) * | 2011-06-09 | 2011-12-21 | 同济大学 | Preparation method of KNN (K0.5Na0.5NbO3)-based piezoelectric texture thick film |
Non-Patent Citations (1)
| Title |
|---|
| 那文菊 等: "(Ba1-xCax)(Ti0.82Zr0.18)O3陶瓷结构与介电性能研究", 《无机材料学报》, vol. 26, no. 6, 30 June 2011 (2011-06-30), pages 656 - 1 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103541014A (en) * | 2013-10-14 | 2014-01-29 | 中国科学院上海硅酸盐研究所 | Lead-free high-voltage active crystal material and preparation method thereof |
| CN106518053A (en) * | 2015-09-10 | 2017-03-22 | 韩国机械研究院 | Crystal orientation template for BaTiO3-based lead-free piezoelectric ceramics and method for fabricating the same |
| CN105418067A (en) * | 2015-12-08 | 2016-03-23 | 天津大学 | Preparation method of barium calcium zirconate titanate lead-free piezoelectric textured ceramic |
| CN107459346A (en) * | 2017-08-11 | 2017-12-12 | 哈尔滨工业大学 | Leadless piezoelectric barium phthalate base textured ceramic of high electric property and its preparation method and application |
| CN107459346B (en) * | 2017-08-11 | 2019-07-02 | 哈尔滨工业大学 | The preparation method and application of the leadless piezoelectric barium phthalate base textured ceramic of high electric property |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102584226B (en) | 2014-06-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101486570B (en) | Leadless piezoelectric structured thick film and preparation thereof | |
| CN105272244B (en) | A kind of potassium niobate sodium-based leadless piezoelectric ceramic and preparation method thereof | |
| CN106554202B (en) | A kind of bismuth laminated bismuth-sodium titanate high temperature piezoceramics and preparation method thereof | |
| CN102531578B (en) | BCT-BZT-BST (Barium calcium titanate-barium zirconate titanate-barium stannate titanate) ternary system lead-free piezoelectric ceramic | |
| CN111302797B (en) | Potassium-sodium niobate-based leadless piezoelectric ceramic and preparation method thereof | |
| CN109626988B (en) | Piezoelectric ceramic material with high piezoelectric response and high Curie temperature and preparation method thereof | |
| CN104628379B (en) | Height-oriented leadless piezoelectric structured ceramic material and its preparation method and application | |
| CN102815939B (en) | Leadless piezoelectric textured ceramic material and preparation method thereof | |
| CN102850050B (en) | Low temperature sintering piezoelectric ceramic material and preparation method thereof | |
| JP2518703B2 (en) | Laminated composite piezoelectric body and manufacturing method thereof | |
| CN102910902B (en) | BNT-BT-BKT-based perovskite system multielement lead-free piezoelectric ceramic and production method thereof | |
| CN102584226B (en) | Barium-calcium-zirconium-titanium leadless piezoelectric textured thick film and preparation method of thick film | |
| CN102167585B (en) | Multielement-doped bismuth titanate group lead-free piezoceramic material and preparation method thereof | |
| CN102503413A (en) | Textured (1-x-y) BNT-xBKT-yKNN ceramic material and preparation method thereof | |
| CN102643090A (en) | PZT (lead zirconate titanate)-based antiferroelectric ceramic material with low curie point and high bidirectional-adjustable dielectric electric field and preparation method thereof | |
| CN110981468A (en) | Preparation method of sodium bismuth titanate-based piezoelectric ceramic | |
| CN101323522A (en) | Leadless piezoelectric ceramics and method for preparing the same | |
| CN110357624B (en) | High-dielectric-constant glass frit modified strontium zirconate doped potassium-sodium niobate lead-free transparent ceramic material and preparation method thereof | |
| KR101333792B1 (en) | Bismuth-based pb-free piezoelectric ceramics and method of fabricating the same | |
| CN102503409A (en) | Tin calcium barium titanate lead-free piezoelectric ceramic and preparation technology thereof | |
| CN101265081A (en) | Ferroelectric ceramic with low-temperature sintering characteristic and its technique and application | |
| CN105732022A (en) | Preparation method of piezoelectric ceramic with high Curie temperature and film thereof | |
| CN115894020B (en) | PMNZT-based piezoelectric ceramic with high piezoelectric coefficient and preparation method and application thereof | |
| CN102584227A (en) | Barium zirconate titanate-barium calcium titanate (BZT-BCT) lead-free piezoelectric ceramic doped with rare earth oxide yttrium | |
| CN105130419B (en) | A kind of high electric field induced strain lead-free piezoceramic material and preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140625 Termination date: 20170105 |