CN1669985A - Fabrication of Textured Piezoelectric Ceramics Using (001) Oriented Flake SrTiO3 as Template Material - Google Patents

Fabrication of Textured Piezoelectric Ceramics Using (001) Oriented Flake SrTiO3 as Template Material Download PDF

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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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CN100447104C (en
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曹明贺
刘韩星
李东亮
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Wuhan University of Technology WUT
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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

Sheet SrTiO with (001) orientation 3For mould material prepares textured piezoelectric ceramic
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、一种织构化压电陶瓷,其特征在于:其主要化学组成是Pb(Mg1/3Nb2/3)O3-xPbTiO3,其中x=0.429~0.538,含有主要化学组成3~20wt%的(001)取向的片状SrTiO3模板材料,具有(001)取向的片状SrTiO3的形貌。1. A textured piezoelectric ceramic, characterized in that its main chemical composition is Pb(Mg 1/3 Nb 2/3 )O 3 -xPbTiO 3 , where x=0.429~0.538, containing 3~ 20wt% (001) oriented flake SrTiO 3 template material has the morphology of (001) oriented flake SrTiO 3 . 2、制备权利要求1所述的织构化压电陶瓷的方法,其特征在于制备步骤为:2. The method for preparing the textured piezoelectric ceramic according to claim 1, characterized in that the preparation steps are: 第1、以Pb(Mg1/3Nb2/3)O3-xPbTiO3粉和(001)取向的片状SrTiO3为起始原料,其中x=0.429~0.538,按照Pb(Mg1/3Nb2/3)O3-xPbTiO3∶SrTiO3=1∶0.03~0.20质量比配料,首先将Pb(Mg1/3Nb2/3)O3-xPbTiO3粉加入无水乙醇和丁酮组成的混合溶剂中,同时加入分散剂三油酸甘油酯,混合球磨20-26小时,然后按所述配料比加入片状SrTiO3模板材料,粘结剂聚乙烯醇缩丁醛,及聚乙二醇和邻苯二甲酸二丁酯混合塑性剂,再混合球磨20-26小时,制得流延浆料;1. Using Pb(Mg 1/3 Nb 2/3 )O 3 -xPbTiO 3 powder and (001) oriented flake SrTiO 3 as starting materials, where x=0.429~0.538, according to Pb(Mg 1/3 Nb 2/3 )O 3 -xPbTiO 3 : SrTiO 3 =1:0.03~0.20 mass ratio ingredients, firstly add Pb(Mg 1/3 Nb 2/3 )O 3 -xPbTiO 3 powder to absolute ethanol and butanone to form In the mixed solvent, add the dispersant glyceryl trioleate at the same time, mix and ball mill for 20-26 hours, then add the flaky SrTiO 3 template material, the binder polyvinyl butyral, and polyethylene glycol Alcohol and dibutyl phthalate are mixed with a plasticizer, and then mixed and ball milled for 20-26 hours to obtain a casting slurry; 第2、取步骤1所得到的浆料抽真空除泡后在玻璃板上流延成型,在溶剂气氛下自然干燥后切片叠层,经过冷等静压后缓慢升温排塑,在3~10wt%聚乙烯醇水溶液中浸泡5~10小时,取出后进行二次加压;2. Take the slurry obtained in step 1 and vacuumize it to defoam, and cast it on a glass plate, dry it naturally under a solvent atmosphere, slice it and stack it, and slowly heat it up and discharge it after cold isostatic pressing. Soak in polyvinyl alcohol aqueous solution for 5-10 hours, take out and pressurize again; 第3、将步骤2所得到的二次加压样品在氩气气氛下热压烧结后,于高温炉空气气氛中烧结,制成织构化压电陶瓷;3. After the secondary pressurized sample obtained in step 2 is hot-pressed and sintered in an argon atmosphere, it is sintered in an air atmosphere of a high-temperature furnace to make a textured piezoelectric ceramic; 其中所述的无水乙醇和丁酮组成的混合溶剂是无水乙醇与丁酮体积比为1~2∶1的混合液,所述加入的分散剂、粘结剂和塑性剂量分别占混合粉料总量的1.00~1.30wt%、2.50~3.00wt%和4.55~5.15wt%;所述的冷等静压的压力为300~500Mpa;二次加压压力为300~600Mpa;所述的热压烧结温度为900~1000℃,烧结时间为0.5~1小时;所述的高温炉空气气氛中烧结温度为1100~1175℃,烧结时间为4~10小时。Wherein said mixed solvent composed of absolute ethanol and methyl ethyl ketone is a mixed solution of absolute alcohol and methyl ethyl ketone with a volume ratio of 1 to 2: 1, and the added dispersant, binder and plastic amount respectively account for the mixed powder 1.00~1.30wt%, 2.50~3.00wt% and 4.55~5.15wt% of the total amount of material; the pressure of the cold isostatic pressing is 300~500Mpa; the secondary pressing pressure is 300~600Mpa; The pressure sintering temperature is 900-1000°C, and the sintering time is 0.5-1 hour; the sintering temperature in the air atmosphere of the high-temperature furnace is 1100-1175°C, and the sintering time is 4-10 hours.
CNB2005100182960A 2005-02-24 2005-02-24 Preparation of textured piezoelectric ceramic using (001) oriented sheet-like SrTiO3 as template material Expired - Fee Related CN100447104C (en)

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CN109553413A (en) * 2019-01-17 2019-04-02 南方科技大学 Textured piezoelectric ceramic and preparation method and application thereof
CN109650888A (en) * 2018-12-27 2019-04-19 哈尔滨工业大学 A kind of high electric property ternary system lead titanate relaxor ferroelectric orientation ceramic of low temperature texture and its preparation method and application

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