CN102584226B - 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 PDF

Info

Publication number
CN102584226B
CN102584226B CN201210002197.3A CN201210002197A CN102584226B CN 102584226 B CN102584226 B CN 102584226B CN 201210002197 A CN201210002197 A CN 201210002197A CN 102584226 B CN102584226 B CN 102584226B
Authority
CN
China
Prior art keywords
thick film
preparation
leadless piezoelectric
template
screen printing
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.)
Expired - Fee Related
Application number
CN201210002197.3A
Other languages
Chinese (zh)
Other versions
CN102584226A (en
Inventor
翟继卫
白王峰
沈波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tongji University
Original Assignee
Tongji University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Tongji University filed Critical Tongji University
Priority to CN201210002197.3A priority Critical patent/CN102584226B/en
Publication of CN102584226A publication Critical patent/CN102584226A/en
Application granted granted Critical
Publication of CN102584226B publication Critical patent/CN102584226B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

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

A kind of barium calcium zirconium titanium leadless piezoelectric structured thick film and preparation method thereof
Technical field
The invention belongs to leadless piezoelectric material material field, be specifically related to a kind of textured method 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 spationautics, medical science and industrial stopper, transverter, sensor.At present widespread use be Pb-based lanthanumdoped zirconate titanates (PZT) the base piezoelectric of the perovskite typed of lead base, as everyone knows, preparation, use and discarded last handling process in plumbum-based 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 have a task of important realistic meaning.
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 Curie temperature is high, all more than 600 DEG C, its piezoelectric property is poor, the d of bismuth-sodium titanate pottery mostly 33only have 60pC/N, and bismuth titanate ceramics only has 20pC/N.Potassium-sodium niobate material density is low, is difficult to sintering.Barium-titanate material research is more ripe, easily sintering, and its piezoelectric property comparison is superior.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 plumbum-based material.Subsequently, the people such as Liwei improve performance by ion doping, have obtained the performance of comparative superiority.But current leadless piezoelectric material material is mainly by doping and the compound performance of improving material.Recent years, many scholars changed performance by the structure of controlling 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 low voltage high frequency, for the condition that provides is provided in unicircuit; On the other hand, have 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, study the more thick-film material such as PZT and BST and be widely used in various piezoelectricity, ferroelectric, pyroelectric electric device, microwave device and microelectronic mechanical system in radio frequency etc.In addition than pottery, thick film is more conducive to the miniaturization of device.But the textured research of piezoelectric mainly concentrates on block materials, thick film is mainly to concentrate on PZT sill, and the research of lead-free piezoelectric thick film is less, and for (Ba, Ca) (Zr, Ti) O 3texture lead-free piezoelectric thick film has not seen reported.
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 prepare a kind of leadless piezoelectric structured thick film of high oriented growth.
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.In above-mentioned chemical general formula, the numeral in the element lower right corner or letter represent the mol ratio of each corresponding element.
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 comprises the following steps:
1) prepare 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) prepare template: adopt BaTiO 3(BT) flaky powder is template.
3) template of acquisition and base-material prepared burden according to a certain percentage and be placed in mortar, adding solvent, grinding 3-5 hour, then adding binding agent to continue to grind 0.5-1.5 hour, making slurry.
4) take out the slurry that makes, use and draw together template and on platinum, carry out silk screen printing, obtain the diaphragm after silk screen printing, the diaphragm after silk screen printing is kept flat to leave standstill and dry, then repeat silk screen printing and baking step 2-6 time; Diaphragm after drying is waited to static pressure processing, 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.
Step 1) in, described BCZT base-material adopts solid reaction process to make, and adopts BaCO 3, CaCO 3, ZrO 2and TiO 2for raw material, take BaCO according to the stoichiometric ratio of Ba, Ca, Zr and Ti element in BCZT base-material 3, CaCO 3, ZrO 2and TiO 2, prepare through batching, batch mixing, precompressed and heat treatment step successively.
Step 3) in, template and base-material are prepared burden according to a certain percentage and are referred to that described template accounts for the 5%-30% of gross weight taking the gross weight of template and base-material as basis, and optimal selection is 20%.
Above-mentioned solvent is dehydrated alcohol; Preferably, the add-on of described solvent is that the gross weight correspondence of 10g template and base-material adds 25-40ml anhydrous ethanol solvent; Adding the best milling time that solvent grinds is 3 hours.
Above-mentioned binding agent is the mixing solutions of Terpineol 350 and ethyl cellulose, and the weight ratio of Terpineol 350 and ethyl cellulose is 10: (1-1.5).
The viscosity of above-mentioned slurry, by the amount control of the binding agent that adds, is dipped into slurry by glass stick, mentions disposed slurry and can connect into suitable viscosity of line.
The meshcount of above-mentioned silk screen printing is 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; When diaphragm after silk screen printing is dried each time, adopt in the baking oven at 110 DEG C constant temperature drying 30 minutes.
When the film of above-mentioned silk screen printing waits static pressure after drying, 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 DEG C, and soaking time is 4-10 hour, and heat-up rate when thermal treatment is 1-3 DEG C/min.Optimal selection is to be incubated 6 hours at 1300 DEG C.Heat-treat condition can produce certain impact to orientation degree.When thermal treatment, preferably in silicon carbide rod furnace, carry out.
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 ceramic industry, and preparation cost is low, technique is simple, be applicable to large batch of suitability for industrialized production.
2, compared with common prior art, textured (Ba xca y) (Zr zti m) O 3lead-free piezoelectric thick film shows good orientation degree, and texture degree can reach 81%, has overcome the low difficult problem of orientation degree in ordinary skill.
3, textured (Ba xca y) (Zr zti m) O 3lead-free piezoelectric thick film does not almost change the Curie temperature of material.
4, (Ba of the present invention xca y) (Zr zti m) O 3leadless piezoelectric structured thick film, for the miniaturization of device, the development of chip type lay 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 the aspects such as piezoelectric transducer, piezoelectric motors and high precision position shift controller, is conducive to the development of the miniaturization of device.
Brief description of the drawings
Fig. 1 is the textured (Ba that in embodiment 1, template content is 5% 0.85ca 0.15) (Zr 0.1ti 0.9) O 3the X ray diffracting spectrum of lead-free piezoelectric thick film.
Textured (the Ba that in Fig. 2 embodiment 2, template content is 20% 0.85ca 0.15) (Zr 0.1ti 0.9) O 3the X ray diffracting spectrum of lead-free piezoelectric thick film.
Textured (the Ba that in Fig. 3 embodiment 3, template content is 30% 0.85ca 0.15) (Zr 0.1ti 0.9) O 3the X ray diffracting spectrum of lead-free piezoelectric thick film.
Textured (the Ba that in Fig. 4 embodiment 2, template content is 20% 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 are only not used in and limit the scope of the invention for the present invention is described.
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 2for raw material, according to (Ba 0.8425ca 0.1575) (Zr 0.105ti 0.895) O 3in base-material, the stoichiometric ratio of Ba, Ca, Zr and Ti element adopts solid reaction process to make.When preparation, raw mixture 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 DEG C, and the time is 4 hours.
Take 0.5g barium titanate template and 9.5g (Ba 0.8425ca 0.1575) (Zr 0.105ti 0.895) O 3base-material is placed in mortar, adds dehydrated alcohol 25ml to grind 3 hours, adds the binding agent preparing to continue to grind 1 hour, and described binding agent is the mixing solutions of Terpineol 350 and ethyl cellulose, and its both weight ratio is 10: 1.Take out the slurry of preparation, choose 200 object plates for screen printing, carry out silk screen printing on platinum sheet, every brush one deck is dried 30 minutes in the baking oven of 110 DEG C, repeatedly in triplicate.Together with film complete silk screen printing is glutinous with aluminum oxide, wait static pressure, 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 DEG C of insulations 6 hours, and temperature rise rate is 2 DEG C/min, 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 be found out and only have Perovskite Phase structure from scheming, and does not observe other dephasigns.By 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 2for raw material, according to (Ba 0.82ca 0.18) (Zr 0.12ti 0.88) O 3in base-material, the stoichiometric ratio of Ba, Ca, Zr and Ti element adopts solid reaction process to make.When preparation, raw mixture 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 DEG C, and the time is 4 hours.
Take 2g barium titanate template and 8g (Ba 0.82ca 0.18) (Zr 0.12ti 0.88) O 3base-material is placed in mortar, adds dehydrated alcohol 25ml to grind 3 hours, adds the binding agent preparing to continue to grind 1 hour, and described binding agent is the mixing solutions of Terpineol 350 and ethyl cellulose, and its both weight ratio is 10: 1.2.Take out the slurry of preparation, choose 200 object plates for screen printing, carry out silk screen printing on platinum sheet, every brush one deck is dried 30 minutes in the baking oven of 110 DEG C, repeatedly in triplicate.Together with the complete film of silk screen printing is glutinous with aluminum oxide, wait static pressure, 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 DEG C of insulations 6 hours, and temperature rise rate is 2 DEG C/min, 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 be found out and only have Perovskite Phase structure from scheming, and does not observe other dephasigns.By X ray diffracting spectrum, Lotgering ' the s factorF=81% calculating, 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 the present embodiment obtains 0.85ca 0.15) (Zr 0.1ti 0.9) O 3lead-free piezoelectric thick film SEM figure, known 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 2for raw material, according to (Ba 0.805ca 0.195) (Zr 0.13ti 0.87) O 3in base-material, the stoichiometric ratio of Ba, Ca, Zr and Ti element adopts solid reaction process to make.When preparation, raw mixture 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 DEG C, and the time is 4 hours.
Take 3g barium titanate template and 7g (Ba 0.805ca 0.195) (Zr 0.13ti 0.87) O 3base-material is placed in mortar, adds dehydrated alcohol 25ml to grind 3 hours, adds the binding agent preparing to continue to grind 1 hour, and described binding agent is the mixing solutions of Terpineol 350 and ethyl cellulose, and its both weight ratio is 10: 1.5.Take out the slurry of preparation, choose 200 object plates for screen printing, carry out silk screen printing on platinum sheet, every brush one deck is dried 30 minutes in the baking oven of 110 DEG C, repeatedly in triplicate.Together with the complete film of silk screen printing is glutinous with aluminum oxide, wait static pressure, 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 DEG C of insulations 6 hours, and temperature rise rate is 2 DEG C/min, 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 be found out and only have Perovskite Phase structure from scheming, and does not observe other dephasigns.By 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
According to the method preparation (Ba of embodiment 2 0.748ca 0.252) (Zr 0.132ti 0.868) O 3base-material.Take 2g barium titanate template and 8g (Ba 0.748ca 0.252) (Zr 0.132ti 0.868) O 3base-material is placed in mortar, adds dehydrated alcohol 25ml to grind 5 hours, adds the binding agent (Terpineol 350 and ethyl cellulose mixing solutions) preparing to continue to grind 1.5 hours.Take out the slurry of preparation, choose 250 object plates for screen printing, carry out silk screen printing on platinum sheet, every brush one deck is dried 30 minutes in the baking oven of 110 DEG C, repeatedly in triplicate.Together with the complete film of silk screen printing is glutinous with aluminum oxide, wait static pressure, pressure is 100MPa.Taking-up waits the good sample of static pressure, in silicon carbide rod furnace, heat-treats, and thermal treatment temp is 1200 DEG C of insulations 10 hours, and temperature rise rate is 1 DEG C/min, 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.
After testing, (the Ba that the 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 only have Perovskite Phase structure, does not observe other dephasigns.By X ray diffracting spectrum, Lotgering ' the s factor F=76% calculating, 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
According to the method preparation (Ba of embodiment 2 0.838ca 0.162) (Zr 0.072ti 0.928) O 3base-material.Take 2g barium titanate template and 8g (Ba 0.838ca 0.162) (Zr 0.072ti 0.928) O 3base-material is placed in mortar, adds dehydrated alcohol 30ml to grind 3 hours, adds the binding agent (Terpineol 350 and ethyl cellulose mixing solutions) preparing to continue to grind 1 hour.Take out the slurry of preparation, choose 150 object plates for screen printing, carry out silk screen printing on platinum sheet, every brush one deck is dried 30 minutes in the baking oven of 110 DEG C, repeatedly repeats four times.Together with the complete film of silk screen printing is glutinous with aluminum oxide, wait static pressure, pressure is 250MPa.Taking-up waits the good sample of static pressure, in silicon carbide rod furnace, heat-treats, and thermal treatment temp is 1400 DEG C of insulations 4 hours, and temperature rise rate is 3 DEG C/min, 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.
After testing, (the Ba that the 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 only have Perovskite Phase structure, does not observe other dephasigns.By X ray diffracting spectrum, Lotgering ' the s factor F=78% calculating, has obtained the good (Ba of orientation degree 0.865ca 0.135) (Zr 0.06ti 0.94) O 3lead-free piezoelectric thick film.

Claims (9)

1. a 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, the barium calcium zirconium titanium leadless piezoelectric structured thick film thickness obtaining is 20-30 μ m;
Described barium calcium zirconium titanium leadless piezoelectric structured thick film is made by the preparation method who mainly comprises the following steps:
1) prepare 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) prepare template: adopt BaTiO 3flaky powder is template;
3) template of acquisition and base-material prepared burden according to a certain percentage and be placed in mortar, adding solvent, grinding 3-5 hour, then adding binding agent to continue to grind 0.5-1.5 hour, making slurry;
4) take out the slurry making, use and draw together template; On platinum, carry out silk screen printing, obtain the diaphragm after silk screen printing, the diaphragm after silk screen printing is kept flat to leave standstill and dry, then repeat silk screen printing and baking step 2-6 time; Diaphragm after drying is waited to static pressure processing, obtain green compact; The green compact that taking-up presses are heat-treated and are obtained described barium calcium zirconium titanium leadless piezoelectric structured thick film.
2. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 1, mainly comprises the following steps:
1) prepare 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) prepare template: adopt BaTiO 3flaky powder is template;
3) template of acquisition and base-material prepared burden according to a certain percentage and be placed in mortar, adding solvent, grinding 3-5 hour, then adding binding agent to continue to grind 0.5-1.5 hour, making slurry;
4) take out the slurry making, use and draw together template; On platinum, carry out silk screen printing, obtain the diaphragm after silk screen printing, the diaphragm after silk screen printing is kept flat to leave standstill and dry, then repeat silk screen printing and baking step 2-6 time; Diaphragm after drying is waited to static pressure processing, obtain green compact; The green compact that taking-up presses are heat-treated and are obtained described 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 step 3), described solvent is dehydrated alcohol; The add-on of described solvent is that the gross weight correspondence of every 10g template and base-material adds 25-40mL dehydrated alcohol.
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 step 3), described binding agent is the mixing solutions of Terpineol 350 and ethyl cellulose, and the weight ratio of Terpineol 350 and ethyl cellulose 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 step 3), template and base-material are prepared burden according to a certain percentage and referred to that described template accounts for the 5%-30% of gross weight taking the gross weight of template and base-material as basis.
6. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 2, is characterized in that, in step 4), the meshcount of described silk screen printing is 100-300 order; Thick film after silk screen printing constant temperature 30 minutes at 110 DEG C.
7. the preparation method of barium calcium zirconium titanium leadless piezoelectric structured thick film as claimed in claim 2, is characterized in that, in step 4), the described pressure that waits static pressure is 100-250MPa; The described dwell time of waiting static pressure 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 step 4), described heat treated temperature is 1200-1400 DEG C, and soaking time is 4-10 hour, and heat-up rate when thermal treatment is 1-3 DEG C/min; When described thermal treatment, in silicon carbide rod furnace, carry out.
9. 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.
CN201210002197.3A 2012-01-05 2012-01-05 Barium-calcium-zirconium-titanium leadless piezoelectric textured thick film and preparation method of thick film Expired - Fee Related CN102584226B (en)

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 CN102584226A (en) 2012-07-18
CN102584226B true 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)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
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
KR101981649B1 (en) * 2015-09-10 2019-05-23 한국기계연구원 Templates for textured 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
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

Citations (2)

* Cited by examiner, † Cited by third party
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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 (2)

* Cited by examiner, † Cited by third party
Title
(Ba1-xCax)(Ti0.82Zr0.18)O3陶瓷结构与介电性能研究;那文菊 等;《无机材料学报》;20110630;第26卷(第6期);第656页左栏第1段 *
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》.2011,第26卷(第6期),第656页左栏第1段.

Also Published As

Publication number Publication date
CN102584226A (en) 2012-07-18

Similar Documents

Publication Publication Date Title
CN105272244B (en) A kind of potassium niobate sodium-based leadless piezoelectric ceramic and preparation method thereof
CN101486570B (en) Leadless piezoelectric structured thick film and preparation 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
CN104628379B (en) Height-oriented leadless piezoelectric structured ceramic material and its preparation method and application
CN109626988B (en) Piezoelectric ceramic material with high piezoelectric response and high Curie temperature and preparation method thereof
CN106554202B (en) A kind of bismuth laminated bismuth-sodium titanate high temperature piezoceramics and preparation method thereof
CN102815939B (en) Leadless piezoelectric textured ceramic material and preparation method thereof
CN110981468B (en) Preparation method of sodium bismuth titanate-based piezoelectric ceramic
CN102167585B (en) Multielement-doped bismuth titanate group lead-free piezoceramic material and preparation method thereof
CN102584226B (en) Barium-calcium-zirconium-titanium leadless piezoelectric textured thick film and preparation method of thick film
CN102503413A (en) Textured (1-x-y) BNT-xBKT-yKNN ceramic material and preparation method thereof
CN102850050A (en) Low temperature sintering piezoelectric ceramic material and preparation method thereof
CN102910905A (en) Low-temperature sintered zirconate-titanate barium calcium based leadless piezoelectric ceramic and preparation method thereof
CN103979955A (en) Barium titanate based leadless piezoceramic material doped and modified by lithium-aluminum ion pair and preparing method thereof
CN110357624B (en) High-dielectric-constant glass frit modified strontium zirconate doped potassium-sodium niobate lead-free transparent ceramic material and preparation method thereof
CN101323522A (en) Leadless piezoelectric ceramics and method for preparing the same
CN109553413A (en) A kind of textured piezoelectric ceramic and its preparation method and application
CN102503409A (en) Tin calcium barium titanate lead-free piezoelectric ceramic and preparation technology thereof
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
CN103880416B (en) Preparation method for sintering sodium bismuth titanate-based lead-free piezoelectric ceramics at low temperature
CN102285797B (en) Preparation method of KNN (K0.5Na0.5NbO3)-based piezoelectric texture thick film
CN104557023A (en) Piezoelectric material
CN103086715A (en) Preparation method of lead zirconate-titanate piezoelectric ceramic powder

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