CN1669985A - Preparation of textured piezoelectric ceramic using (001) oriented sheet-like SrTiO3 as template material - Google Patents
Preparation of textured piezoelectric ceramic using (001) oriented sheet-like SrTiO3 as template material Download PDFInfo
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- CN1669985A CN1669985A CN200510018296.0A CN200510018296A CN1669985A CN 1669985 A CN1669985 A CN 1669985A CN 200510018296 A CN200510018296 A CN 200510018296A CN 1669985 A CN1669985 A CN 1669985A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910002370 SrTiO3 Inorganic materials 0.000 title abstract 4
- 238000005245 sintering Methods 0.000 claims abstract description 74
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 39
- 239000012298 atmosphere Substances 0.000 claims abstract description 24
- 239000011230 binding agent Substances 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 18
- 239000012046 mixed solvent Substances 0.000 claims abstract description 18
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 229910020231 Pb(Mg1/3Nb2/3)O3-xPbTiO3 Inorganic materials 0.000 claims abstract description 8
- 229910020226 Pb(Mg1/3Nb2/3)O3−xPbTiO3 Inorganic materials 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000005266 casting Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 229910002367 SrTiO Inorganic materials 0.000 claims description 40
- 229920003023 plastic Polymers 0.000 claims description 22
- 239000004033 plastic Substances 0.000 claims description 22
- 239000006185 dispersion Substances 0.000 claims description 20
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 19
- 239000011812 mixed powder Substances 0.000 claims description 17
- 238000000465 moulding Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- BAECOWNUKCLBPZ-HIUWNOOHSA-N Triolein Natural products O([C@H](OCC(=O)CCCCCCC/C=C\CCCCCCCC)COC(=O)CCCCCCC/C=C\CCCCCCCC)C(=O)CCCCCCC/C=C\CCCCCCCC BAECOWNUKCLBPZ-HIUWNOOHSA-N 0.000 claims description 3
- PHYFQTYBJUILEZ-UHFFFAOYSA-N Trioleoylglycerol Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(OC(=O)CCCCCCCC=CCCCCCCCC)COC(=O)CCCCCCCC=CCCCCCCCC PHYFQTYBJUILEZ-UHFFFAOYSA-N 0.000 claims description 3
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 3
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000005357 flat glass Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 238000003475 lamination Methods 0.000 claims description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 3
- -1 polyoxyethylene Polymers 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 claims description 3
- 229940117972 triolein Drugs 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 2
- 235000011194 food seasoning agent Nutrition 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 abstract description 2
- 238000009415 formwork Methods 0.000 abstract 2
- 239000012300 argon atmosphere Substances 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 238000010030 laminating Methods 0.000 abstract 1
- 238000010348 incorporation Methods 0.000 description 14
- 238000005056 compaction Methods 0.000 description 13
- 238000001125 extrusion Methods 0.000 description 13
- 239000013078 crystal Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910020215 Pb(Mg1/3Nb2/3)O3PbTiO3 Inorganic materials 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
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Abstract
Disclosed is a method for preparing texture piezoelectric ceramic film wherein the major chemical composition of the ceramics is Pb(Mg1/3Nb2/3)O3-xPbTiO3, x=0.429-0.538, containing 3-20 wt% (001) oriented sheet-like SrTiO3 formwork material, and having the shape of (001) oriented sheet-like SrTiO3. The preparation process comprises charging Pb(Mg1/3Nb2/3)O3-xPbTiO3 powder into the mixed solvent of anhydrous alcohol and methyl ethyl ketone, charging dispersing agent simultaneously, mixing and ball milling, then charging SrTiO3 formwork material, charging binding agent and plasticizing agent simultaneously, mixing and ball milling again, de-soaking the obtained slurry and doctor-blade casting, drying, laminating and press forming, subjecting the samples to isostatic cool pressing and plastic-discharging at elevated temperature, immersing in polyvinyl alcohol aqueous solution and pressurizing again, thermally pressing and sintering at the presence of argon atmosphere, and sintering in the atmosphere of air atmosphere, The prepared textured piezo-electric ceramics has higher degree of orientation and higher piezoelectric constant.
Description
Technical field
The present invention relates to a kind of textured piezoelectric ceramic and preparation method thereof, be specifically related to a kind of sheet SrTiO with (001) orientation
3For mould material prepares Pb (Mg
1/3Nb
2/3) O
3-PbTiO
3The base textured piezoelectric ceramic.
Background technology
Pb (Mg
1/3Nb
2/3) O
3(PMN) basic pottery is typical relaxation sections electric material, is introducing (PbTiO
3) after PT constitutes the PMN-PT binary system, can significantly improve its Curie temperature, be widely used in aspects such as micro positioner, stopper, smart material and device.When PT content was 30-35mol%, there was an accurate homotype phase boundary (MPB) in system, and near the material of prescription this phase boundary has dielectric, piezoelectric property preferably.Though the PMN-PT monocrystalline has preferable performance, because the single crystal growing technical difficulty, at large size, doping vario-property and limited its development in price; Though and traditional PMN-PT polycrystalline ceramics synthesis technique is simple, because crystal grain random alignment in the polycrystalline ceramics, the anisotropy of crystal grain is tending towards equalization on the whole, and performance is cancelled out each other and do not reached the standard of monocrystalline far away.Texturing polycrystalline ceramics by the template grain growth preparation has solved this problem effectively.The texturing polycrystalline material is meant that the crystal plane of each little crystal grain is orientated mutually and is consistent, like this it almost near the performance of monocrystalline, it is also more easy to polarize; Compare with single crystal preparation, reduced its synthetic cost again.
Template grain growth (TGG) is to prepare one of texture ceramic material method commonly used.Its main thought is: the anisotropy template particles of bulk is added in the matrix precursor of ultra-fine grain; Apply shearing force and make the template particles orientation; Make the matrix densification by sintering, create a suitable growing environment to template.The motivating force of TGG process derives from the difference of surface free energy between template particles and the ultra-fine blapharoplast.The present invention is on the basis of TGG method, by behind the plastic removal sample being carried out the secondary pressurization, traditional process system is improved, and the density of stupalith and orientation degree are enhanced.The selection requirement of mould material has similar crystalline structure to body material among the TGG, and suitable shape and thermodynamic stability can be provided.SrTiO
3Be respectively 3.9050 and 4.0166 with the unit cell parameters of PMN-PT, very near and the two be cubic perovskite structure, on structure, SrTiO
3It is comparatively ideal template material of preparation texture type PMN-PT pottery.
Summary of the invention
The purpose of this invention is to provide a kind of textured piezoelectric ceramic, a kind of preparation method of this piezoelectric ceramics is provided simultaneously with high-orientation, high piezoelectric constant.
The present invention adopts by the patent No.: (001) oriented flaky SrTiO of the method preparation of ZL021 15905.X
3Being mould material, is body material (commercial) with PMN-PT, and preparation meets the texturing polycrystalline ceramics of performance requriements.
Its technical scheme is:
A kind of textured piezoelectric ceramic, its main chemical constitution is Pb (Mg
1/3Nb
2/3) O
3-xPbTiO
3, the sheet SrTiO of (001) orientation of main chemical constitution 3～20wt% is contained in x=0.429～0.538 wherein
3Mould material, the sheet SrTiO with (001) orientation
3Pattern.
The preparation process of this textured piezoelectric ceramic is:
1st, with Pb (Mg
1/3Nb
2/3) O
3-x PbTiO
3The sheet SrTiO of powder and (001) orientation
3Be starting raw material, x=0.429～0.538 wherein is according to Pb (Mg
1/3Nb
2/3) O
3-x PbTiO
3: SrTiO
3=1: 0.03～0.20 mass ratio batching is at first with Pb (Mg
1/3Nb
2/3) O
3-x PbTiO
3Powder adds in the mixed solvent of dehydrated alcohol and butanone composition, adds the dispersion agent triolein simultaneously, mixing and ball milling 20-26 hour, adds sheet SrTiO by described ratio of components then
3Mould material, binding agent polyvinyl butyral acetal, and polyoxyethylene glycol and dibutyl phthalate mixing plastic agent, remix ball milling 20-26 hour makes casting slurry;
2nd, get the resulting slurry of step 1 and vacuumize after the de-bubble flow casting molding on sheet glass, the lamination of under solvent atmosphere, cutting into slices after the seasoning, through slow intensification plastic removal after the isostatic cool pressing, in 3～10wt% polyvinyl alcohol water solution, soaked 5～10 hours, carry out the secondary pressurization after the taking-up;
3rd, with the resulting secondary pressurized sample of step 2 behind hot pressed sintering under the argon gas atmosphere, sintering in the High Temperature Furnaces Heating Apparatus air atmosphere is made textured piezoelectric ceramic;
The mixed solvent that wherein said dehydrated alcohol and butanone are formed is that dehydrated alcohol and butanone volume ratio are 1～2: 1 mixed solution, and the dispersion agent of described adding, binding agent and plasticity dosage account for 1.00～1.30wt%, 2.50～3.00wt% and the 4.55～5.15wt% of mixed powder total amount respectively; The pressure of described isostatic cool pressing is 300～500Mpa; The secondary moulding pressure is 300～600Mpa; Described hot pressed sintering temperature is 900～1000 ℃, and sintering time is 0.5～1 hour; Sintering temperature is 1100～1175 ℃ in the described High Temperature Furnaces Heating Apparatus air atmosphere, and sintering time is 4～10 hours.
At this Pb (Mg
1/3Nb
2/3) O
3-x PbTiO
3(PMN-PT) and SrTiO
3In the preparation of mass ratio=1: 0.03～0.20 textured piezoelectric ceramic, our test-results is: work as PbTiO
3Content is near 33% the time, and there is accurate homotype phase boundary in the PMN-PT system that makes with the secondary synthesis method, so body material is selected Pb (Mg for use
1/3Nb
2/3) O
3-33%PbTiO
3, and with this material solid phase method synthetic PMN-PT piezoelectric ceramics constant d
33Be 300pc/N.When the dispersion agent that adds less than 1.00wt%, the PMN-PT powder is difficult to be uniformly dispersed in solvent; When the add-on of dispersion agent surpasses 1.30wt%, the viscosity of slurry is obviously excessive; When the binding agent that adds during less than 2.50wt%, the cohesiveness of slurry is relatively poor, is difficult for bonding between the diaphragm; When the add-on of binding agent surpasses 3.00wt%, dried base substrate is difficult to peel off in substrate; When the add-on of plastic agent less than 4.55wt%, the viscosity of slurry is lower, the snappiness of moulding base is poor; When the add-on of plastic agent surpasses 5.15wt%, between particle owing to form organic bridging increased viscosity; As the SrTiO that mixes
3When mould material surpasses 20wt%, the texturing piezoelectric ceramics constant d of gained
33Because of SrTiO
3Add-on too much reduce to 63pc/N; As the SrTiO that mixes
3During less than 3wt%, do not play directive action preferably because template is very few, its piezoelectric constant also only is 178pc/N; When the hot pressed sintering time less than 0.5 hour, sample does not play the effect of secondary orientation; When the hot pressed sintering time greater than 1 hour, sample descends owing to Pb volatilization makes its piezoelectric property; When sintering temperature was lower than 1100 ℃, the density of pottery significantly descended; When sintering temperature was higher than 1175 ℃, then the fusion burn-off phenomenon appearred in sample, and its piezoelectric property worsens.
The present invention is by control PMN-PT and SrTiO
3SrTiO in mass ratio=1: 0.03～0.20
3Incorporation, the casting slurry of the add-on preparation modest viscosity by regulating organic additive has obtained a kind of textured piezoelectric ceramic with high-orientation, high piezoelectric constant by control moulding process and sintering schedule.The present invention can be used for other manufacturing with texturing stupalith of perovskite structure.
Description of drawings
A among Fig. 1, b are SrTiO
3The scanning electron microscope different amplification photo of mould material
Fig. 2 is the X-ray diffraction analysis figure of texture ceramic and non-texture ceramic sample.
Fig. 3 is the piezoelectric constant (d of texture ceramic and non-texture ceramic
33) comparison diagram
As can be seen from Figure 2, with (001) oriented flaky SrTiO
3As mould material, its (001) orientation degree of texture type piezoelectric ceramics that makes through the TGG method after the improvement technology is significantly improved.
As can be seen from Figure 3, with (001) oriented flaky SrTiO
3As mould material, the piezoelectric property of the texture ceramic that the TGG method after the process improvement technology makes has had improvement clearly than conventional method synthetic pottery.
Embodiment
The embodiment of the invention adopts template crystal grain legal system to be equipped with Pb (Mg
1/3Nb
2/3) O
3-PbTiO
3With SrTiO
3Mass ratio=1: 0.03～0.20 textured piezoelectric ceramic.
Concrete enforcement is as follows: with Pb (Mg
1/3Nb
2/3) O
3-xPbTiO
3(PMN-PT) wherein x=0.429～0.538 powder is a body material, (001) the sheet SrTiO in two step of molten-salt growth method synthetic (method of ZL021 15905.X)
3Be mould material, make textured piezoelectric ceramic by template grain growth.At first the PMN-PT powder being added dehydrated alcohol and butanone volume ratio is in 1～2: 1 mixed solvent of forming, the dispersion agent triolein that adds mixed powder total amount 1.00～1.30wt% simultaneously, mixing and ball milling 20-26 hour, add SrTiO with chemistry than batching then
3Mould material, plastic agent (polyoxyethylene glycol and dibutyl phthalate) remix ball milling 20-26 hour that adds mixed powder total amount 2.50～3.00wt% binding agent polyvinyl butyral acetal and 4.55～5.15wt% simultaneously, the gained slurry is vacuumized after the de-bubble flow casting molding on sheet glass, will mould the compression moulding of base film lamination after the drying.Sample through after the isostatic cool pressing in 550～600 ℃ of slow intensification plastic removals, secondary pressurization after in 3～10wt% polyvinyl alcohol (PVA) aqueous solution, soaking 5～10 hours, 900～1000 ℃ of hot pressed sinterings are after 0.5～1 hour under the argon gas atmosphere, sintering is 4～10 hours under 1100～1175 ℃ of air atmospheres, makes textured piezoelectric ceramic.
This preparation method can be used for other manufacturing with texturing stupalith of perovskite structure.
Preparation Pb (Mg
1/3Nb
2/3) O
3-PbTiO
3The prescription and the following embodiment of condition of base textured piezoelectric ceramic.The X-ray diffraction analysis of ceramics sample is seen Fig. 1, and its (001) of textured piezoelectric ceramic orientation that the TGG method after the process improvement technology obtains the more not pottery of texture is significantly improved; The sample product is ZJ-3A type quasistatic d under room temperature environment
33Its piezoelectric property of test on the survey meter, Fig. 2 is seen in its interpretation of result.
Body material Pb (Mg among the following embodiment
1/3Nb
2/3) O
3-xPbTiO
3. wherein x=0.429～0.538 is commercial product
Embodiment 1,
Press Pb (Mg
1/3Nb
2/3) O
3-0.429PbTiO
3+ SrTiO
3=96.54wt%+3.46wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 1: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.10wt%, 2.64wt%, the 4.65wt% of mixed powder total amount, cold isostatic compaction pressure is 300MPa, soaked 5 hours among the 3wt%PVA, secondary extrusion forming pressure is 300MPa, 900 ℃ of hot pressed sintering temperature, sintering time 0.5 hour; Sintering temperature is 1150 ℃ under the air atmosphere, and sintering time is 4 hours.
Embodiment 2,
Press Pb (Mg
1/3Nb
2/3) O
3-0.429PbTiO
3+ SrTiO
3=95.00wt%+5.00wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 2: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.20wt%, 2.70wt%, the 4.82wt% of mixed powder total amount, cold isostatic compaction pressure is 400MPa, soaked 5 hours among the 4wt%PVA, secondary extrusion forming pressure is 350MPa, 950 ℃ of hot pressed sintering temperature, sintering time 0.5 hour; Sintering temperature is 1150 ℃ under the air atmosphere, and sintering time is 6 hours.
Embodiment 3,
Press Pb (Mg
1/3Nb
2/3) O
3-0.429PbTiO
3+ SrTiO
3=93.50wt%+6.50wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 1.5: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.15wt%, 2.85wt%, the 4.82wt% of mixed powder total amount, cold isostatic compaction pressure is 400MPa, soaked 8 hours among the 5wt%PVA, secondary extrusion forming pressure is 400MPa, 1000 ℃ of hot pressed sintering temperature, sintering time 0.5 hour; Sintering temperature is 1150 ℃ under the air atmosphere, and sintering time is 6 hours.
Embodiment 4,
Press Pb (Mg
1/3Nb
2/3) O
3-0.429PbTiO
3+ SrTiO
3=92.50wt%+7.50wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 2: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.17wt%, 2.90wt%, the 5.00wt% of mixed powder total amount, cold isostatic compaction pressure is 450MPa, soaked 6 hours among the 5wt%PVA, secondary extrusion forming pressure is 450MPa, 950 ℃ of hot pressed sintering temperature, sintering time 1 hour; Sintering temperature is 1150 ℃ under the air atmosphere, and sintering time is 8 hours.
Embodiment 5,
Press Pb (Mg
1/3Nb
2/3) O
3-0.429PbTiO
3+ SrTiO
3=91.50wt%+8.50wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 2: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.25wt%, 2.92wt%, the 5.00wt% of mixed powder total amount, cold isostatic compaction pressure is 400MPa, soaked 5 hours among the 8wt%PVA, secondary extrusion forming pressure is 600MPa, 900 ℃ of hot pressed sintering temperature, sintering time 1 hour; Sintering temperature is 1175 ℃ under the air atmosphere, and sintering time is 4 hours.
Embodiment 6,
Press Pb (Mg
1/3Nb
2/3) O
3-0.538PbTiO
3+ SrTiO
3=90.00wt%+10.00wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 1.5: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.17wt%, 2.83wt%, the 4.99wt% of mixed powder total amount, cold isostatic compaction pressure is 500MPa, soaked 10 hours among the 5wt%PVA, secondary extrusion forming pressure is 500MPa, 950 ℃ of hot pressed sintering temperature, sintering time 0.5 hour; Sintering temperature is 1150 ℃ under the air atmosphere, and sintering time is 8 hours.
Embodiment 7,
Press Pb (Mg
1/3Nb
2/3) O
3-0.538PbTiO
3+ SrTiO
3=88.50wt%+11.50wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 1: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.30wt%, 2.68wt%, the 5.05wt% of mixed powder total amount, cold isostatic compaction pressure is 400MPa, soaked 10 hours among the 8wt%PVA, secondary extrusion forming pressure is 400MPa, 1000 ℃ of hot pressed sintering temperature, sintering time 0.5 hour; Sintering temperature is 1125 ℃ under the air atmosphere, and sintering time is 8 hours.
Embodiment 8,
Press Pb (Mg
1/3Nb
2/3) O
30.429PbTiO
3+ SrTiO
3=87.35wt%+12.65wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 2: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.15wt%, 2.90wt%, the 5.10wt% of mixed powder total amount, cold isostatic compaction pressure is 400MPa, soaked 5 hours among the 10wt%PVA, secondary extrusion forming pressure is 500MPa, 950 ℃ of hot pressed sintering temperature, sintering time 1 hour; Sintering temperature is 1150 ℃ under the air atmosphere, and sintering time is 6 hours.
Embodiment 9,
Press Pb (Mg
1/3Nb
2/3) O
3-0.538PbTiO
3+ SrTiO
3=86.20wt%+13.80wt% batching, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.20wt%, 2.80wt%, the 5.00wt% of mixed powder total amount, cold isostatic compaction pressure is 400MPa, soaked 8 hours among the 10wt%PVA, secondary extrusion forming pressure is 550MPa, 950 ℃ of hot pressed sintering temperature, sintering time 0.5 hour; Sintering temperature is 1150 ℃ under the air atmosphere, and sintering time is 6 hours.
Embodiment 10,
Press Pb (Mg
1/3Nb
2/3) O
3-0.429PbTiO
3+ SrTiO
3=85.00wt%+1 5.00wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 2: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.18wt%, 2.70wt%, the 5.15wt% of mixed powder total amount, cold isostatic compaction pressure is 400MPa, soaked 10 hours among the 8wt%PVA, secondary extrusion forming pressure is 500MPa, 1000 ℃ of hot pressed sintering temperature, sintering time 0.5 hour; Sintering temperature is 1150 ℃ under the air atmosphere, and sintering time is 4 hours.
Embodiment 11,
Press Pb (Mg
1/3Nb
2/3) O
3-0.538PbTiO
3+ SrTiO
3=83.55wt%+16.45wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 2: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.20wt%, 2.83wt%, the 4.83wt% of mixed powder total amount, cold isostatic compaction pressure is 400MPa, soaked 10 hours among the 6wt%PVA, secondary extrusion forming pressure is 500MPa, 950 ℃ of hot pressed sintering temperature, sintering time 0.5 hour; Sintering temperature is 1150 ℃ under the air atmosphere, and sintering time is 8 hours.
Embodiment 12,
Press Pb (Mg
1/3Nb
2/3) O
3-0.538PbTiO
3+ SrTiO
3=82.50wt%+1 7.50wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 2: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.25wt%, 2.80wt%, the 4.70wt% of mixed powder total amount, cold isostatic compaction pressure is 400MPa, soaked 10 hours among the 4wt%PVA, secondary extrusion forming pressure is 500MPa, 950 ℃ of hot pressed sintering temperature, sintering time 1 hour; Sintering temperature is 1130 ℃ under the air atmosphere, and sintering time is 6 hours.
Embodiment 13,
Press Pb (Mg
1/3Nb
2/3) O
3-0.538PbTiO
3+ SrTiO
3=80.00wt%+20.00wt% batching, adopting dehydrated alcohol and butanone volume ratio is the mixed solvent of forming at 2: 1, the incorporation of dispersion agent, binding agent and plastic agent is respectively 1.12wt%, 2.75wt%, the 5.10wt% of mixed powder total amount, cold isostatic compaction pressure is 400MPa, soaked 10 hours among the 5wt%PVA, secondary extrusion forming pressure is 500MPa, 950 ℃ of hot pressed sintering temperature, sintering time 0.5 hour; Sintering temperature is 1150 ℃ under the air atmosphere, and sintering time is 8 hours.
Claims (2)
1, a kind of textured piezoelectric ceramic is characterized in that: its main chemical constitution is Pb (Mg
1/3Nb
2/3) O
3-xPbTiO
3, the sheet SrTiO of (001) orientation of main chemical constitution 3～20wt% is contained in x=0.429～0.538 wherein
3Mould material, the sheet SrTiO with (001) orientation
3Pattern.
2, the method for preparing the described textured piezoelectric ceramic of claim 1 is characterized in that preparation process is:
1st, with Pb (Mg
1/3Nb
2/3) O
3-xPbTiO
3The sheet SrTiO of powder and (001) orientation
3Be starting raw material, x=0.429～0.538 wherein is according to Pb (Mg
1/3Nb
2/3) O
3-xPbTiO
3: SrTiO
3=1: 0.03～0.20 mass ratio batching is at first with Pb (Mg
1/3Nb
2/3) O
3-xPbTiO
3Powder adds in the mixed solvent of dehydrated alcohol and butanone composition, adds the dispersion agent triolein simultaneously, mixing and ball milling 20-26 hour, adds sheet SrTiO by described ratio of components then
3Mould material, binding agent polyvinyl butyral acetal, and polyoxyethylene glycol and dibutyl phthalate mixing plastic agent, remix ball milling 20-26 hour makes casting slurry;
2nd, get the resulting slurry of step 1 and vacuumize after the de-bubble flow casting molding on sheet glass, the lamination of under solvent atmosphere, cutting into slices after the seasoning, through slow intensification plastic removal after the isostatic cool pressing, in 3～10wt% polyvinyl alcohol water solution, soaked 5～10 hours, carry out the secondary pressurization after the taking-up;
3rd, with the resulting secondary pressurized sample of step 2 behind hot pressed sintering under the argon gas atmosphere, sintering in the High Temperature Furnaces Heating Apparatus air atmosphere is made textured piezoelectric ceramic;
The mixed solvent that wherein said dehydrated alcohol and butanone are formed is that dehydrated alcohol and butanone volume ratio are 1～2: 1 mixed solution, and the dispersion agent of described adding, binding agent and plasticity dosage account for 1.00～1.30wt%, 2.50～3.00wt% and the 4.55～5.15wt% of mixed powder total amount respectively; The pressure of described isostatic cool pressing is 300～500Mpa; The secondary moulding pressure is 300～600Mpa; Described hot pressed sintering temperature is 900～1000 ℃, and sintering time is 0.5～1 hour; Sintering temperature is 1100～1175 ℃ in the described High Temperature Furnaces Heating Apparatus air atmosphere, and sintering time is 4～10 hours.
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| CN1585150A (en) * | 2004-05-27 | 2005-02-23 | 上海交通大学 | Growth of ferroelectric thick films with films as seeds by liquid phase epitaxy |
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| CN105121538A (en) * | 2013-04-18 | 2015-12-02 | 国立里昂应用科学学院 | Method for manufacturing composite material which is polarizable under the action of a weak electric field |
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| CN109553413B (en) * | 2019-01-17 | 2021-07-16 | 南方科技大学 | Textured piezoelectric ceramic and preparation method and application thereof |
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