CN104961455A - Texturing piezoelectric ceramic material and preparation method thereof - Google Patents
Texturing piezoelectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a texturing piezoelectric ceramic material and a preparation method thereof. The piezoelectric ceramic material consists of template material crystals and a base body material; the Bi4Ti3O12, Na0.5Bi4.5Ti4O15 or Na0.5Bi0.5TiO3 template material crystals with orientation 001 form direction arrangement in the base body material; the base body material has the following chemical expression: (1-x)Bi0.5Na0.5TiO3-xBaTiO3, and x is ranged from 0.03-0.09. The preparation method for the texturing piezoelectric ceramic material comprises the following steps: preparing base body material thin sheets, coating the surface of the base body material with the template material crystals to form the direction arrangement, stacking a plurality of thin sheets, and performing thermal press forming and sintering to obtain the texturing piezoelectric ceramic material. The preparation method is easy to operate, low in cost and suitable for large-scale industrial production; the prepared piezoelectric ceramic material is high in texturing degree, has the Curie temperature being more than 300 DEG C, is high in piezoelectric property and can be widely applied to the aspects of piezoelectric sensors, piezoelectric motors, high-precision displacement control and the like.
Description
Technical field
The present invention relates to a kind of textured piezoelectric ceramic material and preparation method thereof, belong to leadless piezoelectric material material field.
Background technology
Piezoelectric ceramics is widely used in the fields such as Industry Control, environmental monitoring, communication, infosystem and medicine equipment as sensor, stopper and frequency transformer.The piezoelectric of current widespread use mainly has the PZT (PbZrO of perovskite structure
3-PbTiO
3) and PT (PbTiO
3) material.
Along with people are to the raising day by day of environmental protection consciousness, a lot of countries and regions control more strict to the lead tolerance of electron device, and have proposed unleaded schedule, and this just needs exploitation to substitute PZT (PbZrO
3-PbTiO
3) and PT (PbTiO
3) lead-free piezoceramic material.At present, leadless piezoelectric material material system mainly comprises KNN (Ka
0.5na
0.5nbO
3), BNT (Na
0.5bi
0.5tiO
3), BT (BaTiO
3) and high temperature bismuth laminate ceramic system.The people such as Jaffe find Pb (Zr, Ti) O
3(PZT) pottery shows excellent electric property a narrow Composition Region, and this region is the line of delimitation of cubic phase region and water chestnut side's phase region, and is named as accurate homotype phase boundary (MPB).This concept is introduced leadless piezoelectric field, finds a series of composite ceramic material with high tension performance thus.But the piezoelectric property of this material system does not obtain the raising of essence.
Recent study shows, crystal grain in piezoelectric ceramics is (pottery that in crystal grain, crystallographic axis arranges in a certain direction is called " grain orientation " or " texturing ") after a direction oriented growth, its performance can increase substantially than the performance of crystal grain free growth pottery, about 2 times of crystal grain free growth pottery can be reached, 60% ~ 80% of same component monocrystalline performance, and there is the advantage that preparation time is short, cost is low, be described as " monocrystalline of the poor ".The piezoelectric ceramics grain orientation growing technology be widely used in recent years mainly comprises directional solidification technique, multilayer grain growing technology, templated grain growth and reaction template grain growing technology.Wherein the sample orientation degree prepared of templated grain growth (TGG) and reaction template grain growing technology (RTGG) is high, is widely used in the piezoelectric ceramics preparing oriented growth.Traditional templated grain growth is mainly realized by the technique of flow casting molding, and its main drawback is that the mixing time of casting slurry is long, is unfavorable for large-scale industrial production.
Summary of the invention
An object of the present invention is to be to provide one to have more than 300 DEG C Curie temperature, and the piezoceramic material without lead-type highly-texturedization that piezoelectric property is good.
Another object of the present invention be to provide a kind of simple to operate, cost is low, be applicable to the method for the texturing textured piezoelectric ceramic material described in large-scale industrial production preparation.
The invention provides a kind of textured piezoelectric ceramic material, this textured piezoelectric ceramic material is made up of mould material crystal and body material compound, has the Bi of 001 orientation
4ti
3o
12, Na
0.5bi
4.5ti
4o
15or Na
0.5bi
0.5tiO
3mould material crystal is formed and aligns in body material; Described body material has following chemical expression: (1-x) Bi
0.5na
0.5tiO
3-xBaTiO
3, x is 0.03 ~ 0.09; Described mould material is 1% ~ 30% of base-material quality.
In preferred textured piezoelectric ceramic material, mould material is 5% ~ 15% of body material quality.
In preferred textured piezoelectric ceramic material, in chemical expression, x is 0.05 ~ 0.07.
Present invention also offers a kind of preparation method of described textured piezoelectric ceramic material, this preparation method comprises the following steps:
Step one: prepare mould material crystal and body material thin slice
1), be there is by molten-salt growth method synthesis the Bi of 001 crystalline structure
4ti
3o
12, Na
0.5bi
4.5ti
4o
15or Na
0.5bi
0.5tiO
3mould material;
2), by solid reaction process, hydrothermal method, molten-salt growth method or sol-gel method preparation (1-x) Bi
0.5na
0.5tiO
3-xBaTiO
3body material powder, then by gained body material powder successively through visco-plasticity complete processing and calendering technology process, obtain thickness and be not more than 100 μm of body material thin slices;
Step 2: prepare textured piezoelectric ceramic body of material
In organic solvent, is mixed with slurry by crystalline dispersion for mould material obtained for step one, gained slurry is coated to step one gained body material slice surfaces by painting way forms one deck at body material slice surfaces and has the mould material crystal layer aligned; Again by polylith be coated be brushed with mould material crystal layer body material thin slice superposition, hot-forming, obtain textured piezoelectric ceramic body of material;
Step 3: prepare textured piezoelectric ceramic material
By step 2 gained textured piezoelectric ceramic body of material by intensification binder removal, isostatic sintering, obtained textured piezoelectric ceramic material.
The preparation method of textured piezoelectric ceramic material of the present invention also comprises following preferred version:
Be there is by molten-salt growth method preparation in preferred preparation method the Bi of 001 crystalline structure
4ti
3o
12mould material process is: by Bi
2o
3and TiO
2powder is mixed by wet ball-milling with fused salt, dry after, under being placed in 850 ~ 1150 DEG C of high temperature, be incubated 0.5 ~ 6 hour, products therefrom through washing, oven dry, to obtain final product.
Be there is by molten-salt growth method preparation in preferred preparation method the Na of 001 crystalline structure
0.5bi
4.5ti
4o
15mould material process is: by Na
2cO
3, TiO
2powder, there is the Bi of 001 crystalline structure
4ti
3o
12mould material is mixed by wet ball-milling with fused salt, dry after, under being placed in 800 ~ 1100 DEG C of high temperature, be incubated 1 ~ 8 hour, products therefrom through washing, oven dry, to obtain final product.
Be there is by molten-salt growth method preparation in preferred preparation method the Na of 001 crystalline structure
0.5bi
0.5tiO
3mould material process is: by Na
2cO
3, TiO
2powder, there is the Na of 001 crystalline structure
0.5bi
4.5ti
4o
15mould material is mixed by wet ball-milling with fused salt, dry after, under being placed in 800 ~ 1100 DEG C of high temperature, be incubated 1 ~ 10 hour, products therefrom through washing, oven dry, to obtain final product.
In preferred preparation method, fused salt is NaCl and/or KCl; Most preferably be NaCl.
The solvent that in preferred preparation method, wet ball-milling adopts is dehydrated alcohol.
Adopting scraper or hairbrush to apply a shearing force to the mould material crystal in slurry in preferred preparation method in step 2 in painting process, making mould material crystal at body material slice surfaces in aligning.
Hot-forming in preferred preparation method is the pressure applying a 1 ~ 30MPa in body material thin slice superposition vertical direction, suppresses at 40 ~ 100 DEG C of temperature.Most preferably be the pressure applying a 5 ~ 10MPa in body material thin slice superposition vertical direction, suppress at 60 ~ 80 DEG C of temperature.
Sintering temperature in preferred preparation method is 1050 ~ 1250 DEG C, and the time is 1 ~ 50h.Most preferably be at 1150 ~ 1175 DEG C, sintering 20 ~ 50h.
The Bi adopted in preferred preparation method
2o
3, TiO
2, Na
2cO
3,baCO
3, the raw material such as NaCl and KCl is all commercially available analytical pure raw material.
The organic solvent adopted in step one in preferred preparation method is ethanol.
Before being superposed by polylith body material thin slice in preferred preparation method, body material thin slice is cut into suitable size.
In preferred preparation method, dump temperature is 500 ~ 700 DEG C; Most preferably be 580 ~ 620 DEG C.
When the body material thin slice that painting of the present invention is brushed with mould material crystal layer superposes, select suitable thin slice block number according to desired thickness.The body material thin slice painting of some amount being brushed with mould material crystal layer is added to certain height, then mould is put into, and on die coat one can the heating unit of regulating and controlling temperature, then this is added with the mould of heating unit as under single shaft tabletting machine, heating, again heat-insulating pressurizing, make to be bonded together the textured piezoelectric ceramic body of material forming compact structure between thin slice and thin slice.
Described (1-x) Bi
0.5na
0.5tiO
3-xBaTiO
3the preparation method of body material is preferably solid reaction process.Described solid phase method is: by Na
2cO
3, Bi
2o
3and TiO
2powder raw material obtains slurry in organic solvent by Ball milling, and gained slurry is dried, and pre-burning, carries out secondary ball milling, dries further, grinds, to obtain final product.Described calcined temperature is 750 ~ 950 DEG C, and burn-in time is 2 ~ 4h; Preferred calcined temperature is 840 ~ 860 DEG C, burn-in time is 1 ~ 3h.Described ball milling and the time of secondary ball milling are 24h.
The thickness range that textured piezoelectric ceramic material is being not more than 50mm obtained in preferred preparation method is controlled.
Beneficial effect of the present invention: a) preparation method of textured piezoelectric ceramic material of the present invention is simple to operate, production cost is low, is applicable to large batch of suitability for industrialized production; B) (1-x) Bi in obtained textured piezoelectric ceramic material
0.5na
0.5tiO
3-xBaTiO
3ceramic crystalline grain grows all in a certain direction, changes the deficiency of the orientation of ordinary sinter ceramic crystalline grain thing, makes pottery in performance close to the performance that monocrystalline has; C) obtained textured piezoelectric ceramic material, texture degree is up to 94%, and Curie temperature is more than 300 DEG C, and electric field induced strain performance can reach 0.5% (60kV/cm), and being roughly equal to dynamic piezoelectric coefficient is 537pm/V.D) the textured piezoelectric ceramic material that the present invention obtains has good application prospect in piezoelectric transducer, piezoelectric motors and high precision displacement control etc., advances the application progress of high electric field induced strain material.
Accompanying drawing explanation
The Bi that [Fig. 1] obtains for embodiment 1
4ti
3o
12the scanning electron microscope (SEM) photograph of mould material.
The Bi that [Fig. 2] obtains for embodiment 1
4ti
3o
12the XRD figure of mould material.
The Na that [Fig. 3] obtains for embodiment 2
0.5bi
4.5ti
4o
15the scanning electron microscope (SEM) photograph of mould material.
The Na that [Fig. 4] obtains for embodiment 2
0.5bi
4.5ti
4o
15the XRD figure of mould material.
The Na that [Fig. 5] obtains for embodiment 3
0.5bi
0.5tiO
3the scanning electron microscope (SEM) photograph of mould material.
The Na that [Fig. 6] obtains for embodiment 3
0.5bi
0.5tiO
3the XRD figure of mould material.
The scanning electron microscope (SEM) photograph of the 0.93BNT-0.07BT stupalith that [Fig. 7] obtains for embodiment 3.
Embodiment
Technical scheme of the present invention is further described below by specific embodiment.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.
Embodiment 1
Preparation is with Bi
4ti
3o
12for the texturing 0.93BNT-0.07BT pottery of template.
Take 11.356g Bi
2o
3powder, 2.607g TiO
2powder, then take 15.358g NaCl powder, by all powders and dehydrated alcohol ball milling mixing and ball milling 24 hours, mixed material is dried, load alumina crucible and put into 1100 DEG C, stove insulation 2 hours, put into Büchner funnel deionized water after cooling and clean NaCl, dry and obtain sheet Bi
4ti
3o
12template.Visco-plasticity complete processing (VPP) and calendering technology is used to obtain the 0.93BNT-0.07BT thin slice green compact that thickness is not more than 100 μm; By Bi
4ti
3o
12one in mould material is distributed in alcohol or other organic solvents, is made into the slurry of high density; With hairbrush or other instruments surface brush one deck template inculating crystal layer at 0.93BNT-0.07BT green chip; By hot-forming for lamination after diaphragm cutting; Sintering after sticky for base substrate row after shaping, isostatic pressed is obtained textured 0.93BNT-0.07BT stupalith, and its texture degree is 78%.
It is obvious sheet structure that Fig. 1 describes prepared bismuth titanates, and most of sheet size reach more than 10 microns illustrate 1000 DEG C of temperature make template obtain growing up more fully.
The sheet mould material thing that Fig. 2 describes synthesis is single bismuth titanates thing phase mutually, and the template of gained is pure bismuth titanates template.
Embodiment 2
Preparation is with Na
0.5bi
4.5ti
4o
15for the texturing 0.93BNT-0.07BT pottery of template.
With Na
2cO
3powder, TiO
2powder, sheet Bi
4ti
3o
12presoma and fused salt are raw material, take raw material according to certain stoichiometric ratio, the quality of fused salt and Na
2cO
3powder, TiO
2powder, sheet Bi
4ti
3o
12the total mass of presoma is equal; All raw materials are carried out wet ball-milling mixing post-drying, then in 1050 DEG C of insulations 4 hours, finally clean residual fused salt with deionized water, dry and obtain sheet Na
0.5bi
4.5ti
4o
15template.Visco-plasticity complete processing (VPP) and calendering technology is used to obtain the 0.93BNT-0.07BT thin slice green compact that thickness is not more than 100 μm; By Na
0.5bi
4.5ti
4o
15or Na
0.5bi
0.5tiO
3one in mould material is distributed in alcohol or other organic solvents, is made into the slurry of high density; With hairbrush or other instruments surface brush one deck template inculating crystal layer at 0.93BNT-0.07BT green chip; By hot-forming for lamination after diaphragm cutting; Sintering after sticky for base substrate row after shaping, isostatic pressed is obtained textured 0.93BNT-0.07BT stupalith, and its texture degree is 80%.
Gained ceramic material sample being worn into thickness is 0.45mm thin slice, thin slice upper and lower surface by Ag electrode, at room temperature in silicone oil, test the performance of described textured 0.93BNT-0.07BT pottery, its electric field induced strain is up to 0.5% (60kV/cm), and dynamic piezoelectric coefficient is 475pm/V.
Fig. 3 describes prepared Na
0.5bi
4.5ti
4o
15seed crystal is obvious sheet structure, and most of sheet size reach more than 10 microns illustrate 1000 DEG C of temperature make template obtain growing up more fully.
The sheet mould material thing that Fig. 4 describes synthesis is single Na mutually
0.5bi
4.5ti
4o
15thing phase, the template of gained is pure Na
0.5bi
4.5ti
4o
15template.
Embodiment 3
Preparation is with Na
0.5bi
0.5tiO
3for the texturing 0.93BNT-0.07BT pottery of template.
Visco-plasticity complete processing (VPP) and calendering technology is used to obtain (1-x) BNT-xBT thin slice green compact that thickness is not more than 100 μm; By Na
0.5bi
0.5tiO
3one in mould material is distributed in alcohol or other organic solvents, is made into the slurry of high density; With hairbrush or other instruments surface brush one deck template inculating crystal layer at (1-x) BNT-xBT green chip; By hot-forming for lamination after diaphragm cutting; Sintering after sticky for base substrate row after shaping, isostatic pressed is obtained textured (1-x) BNT-xBT stupalith, and its texture degree is 94%.
Gained ceramic material sample being worn into thickness is 0.45mm thin slice, thin slice upper and lower surface by Ag electrode, at room temperature in silicone oil, test the performance of described textured 0.93BNT-0.07BT pottery, its electric field induced strain is 0.32% (60kV/cm), and dynamic piezoelectric coefficient is 537pm/V.
Fig. 5 describes prepared Na
0.5bi
0.5tiO
3seed crystal is obvious sheet structure, and most of sheet size reach more than 10 microns illustrate 1000 DEG C of temperature make template obtain growing up more fully.Fig. 6 can find out that there is very high diffracted intensity at the peak in (100) and (200) direction, but not the peak diffracted intensity in (100) and (200) direction is very low, describe the ceramic orientation created clearly of 0.93BNT-0.07BT, create high texture degree.
Fig. 7 can find out that prepared 0.93BNT-0.07BT pottery is all sheet structure, and proper alignment in a certain direction, illustrate sheet structure obviously and sheet unanimously lie down, create high texture degree.
As can be seen from embodiment 1 ~ 3: it is 0.45mm thin slice that ceramic material sample obtained for embodiment 1 ~ 3 is worn into thickness, thin slice upper and lower surface by Ag electrode, in room temperature silicone oil, its electric field induced strain is tested under the voltage of 60kV/cm, when template content is 20%, texture degree is up to 94%, but now because chemical composition skew causes electric field induced strain performance lower.When template content is 5%, texture degree reaches 70% electric field induced strain performance is 0.5% (60kV/cm), and dynamic piezoelectric coefficient is 537pm/V.This shows that the orientation of crystal grain and chemical composition determine ceramic electric field induced strain performance, although the texture degree of pottery does not reach maximum value when template content is 5%, now achieves optimum performance.
Claims (10)
1. a textured piezoelectric ceramic material, is made up of mould material crystal and body material compound, it is characterized in that, have the Bi of 001 orientation
4ti
3o
12, Na
0.5bi
4.5ti
4o
15or Na
0.5bi
0.5tiO
3mould material crystal is formed and aligns in body material;
Described body material has following chemical expression: (1-x) Bi
0.5na
0.5tiO
3-xBaTiO
3, x is 0.03 ~ 0.09;
Described mould material is 1% ~ 30% of base-material quality.
2. textured piezoelectric ceramic material as claimed in claim 1, it is characterized in that, described mould material is 5% ~ 15% of body material quality.
3. textured piezoelectric ceramic material as claimed in claim 1, it is characterized in that, in chemical expression, x is 0.05 ~ 0.07.
4. the preparation method of the textured piezoelectric ceramic material described in any one of claims 1 to 3, is characterized in that, comprise the following steps:
Step one: prepare mould material crystal and body material thin slice
1), be there is by molten-salt growth method synthesis the Bi of 001 crystalline structure
4ti
3o
12, Na
0.5bi
4.5ti
4o
15or Na
0.5bi
0.5tiO
3mould material;
2), by solid reaction process, hydrothermal method, molten-salt growth method or sol-gel method preparation (1-x) Bi
0.5na
0.5tiO
3-xBaTiO
3body material powder, then by gained body material powder successively through visco-plasticity complete processing and calendering technology process, obtain thickness and be not more than 100 μm of body material thin slices;
Step 2: prepare textured piezoelectric ceramic body of material
In organic solvent, is mixed with slurry by crystalline dispersion for mould material obtained for step one, gained slurry is coated to step one gained body material slice surfaces by painting way forms one deck at body material slice surfaces and has the mould material crystal layer aligned; Again by polylith be coated be brushed with mould material crystal layer body material thin slice superposition, hot-forming, obtain textured piezoelectric ceramic body of material;
Step 3: prepare textured piezoelectric ceramic material
By step 2 gained textured piezoelectric ceramic body of material by intensification binder removal, isostatic sintering, obtained textured piezoelectric ceramic material.
5. preparation method as claimed in claim 4, is characterized in that, is had the Bi of 001 crystalline structure by molten-salt growth method preparation
4ti
3o
12mould material process is: by Bi
2o
3and TiO
2powder is mixed by wet ball-milling with fused salt, dry after, under being placed in 850 ~ 1150 DEG C of high temperature, be incubated 0.5 ~ 6 hour, products therefrom through washing, oven dry, to obtain final product;
Be there is by molten-salt growth method preparation the Na of 001 crystalline structure
0.5bi
4.5ti
4o
15mould material process is: by Na
2cO
3, TiO
2powder, there is the Bi of 001 crystalline structure
4ti
3o
12mould material is mixed by wet ball-milling with fused salt, dry after, under being placed in 800 ~ 1100 DEG C of high temperature, be incubated 1 ~ 8 hour, products therefrom through washing, oven dry, to obtain final product;
Be there is by molten-salt growth method preparation the Na of 001 crystalline structure
0.5bi
0.5tiO
3mould material process is: by Na
2cO
3, TiO
2powder, there is the Na of 001 crystalline structure
0.5bi
4.5ti
4o
15mould material is mixed by wet ball-milling with fused salt, dry after, under being placed in 800 ~ 1100 DEG C of high temperature, be incubated 1 ~ 10 hour, products therefrom through washing, oven dry, to obtain final product.
6. preparation method as claimed in claim 5, it is characterized in that, described fused salt is NaCl and/or KCl.
7. preparation method as claimed in claim 4, is characterized in that, adopting scraper or hairbrush to apply a shearing force to the mould material crystal in slurry in painting process, making mould material crystal at body material slice surfaces in aligning in step 2.
8. preparation method as claimed in claim 4, is characterized in that, described hot-forming be the pressure applying a 1 ~ 30MPa in body material thin slice superposition vertical direction, suppress at 40 ~ 100 DEG C of temperature.
9. preparation method as claimed in claim 4, it is characterized in that, described sintering temperature is 1050 ~ 1250 DEG C, and the time is 1 ~ 50h.
10. preparation method as claimed in claim 4, is characterized in that, (1-x) Bi
0.5na
0.5tiO
3-xBaTiO
3body material is obtained by solid reaction process.
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| CN104402432A (en) * | 2014-10-29 | 2015-03-11 | 中南大学 | Textured piezoelectric ceramic material and preparation method thereof |
| CN107326432B (en) * | 2017-06-30 | 2019-07-02 | 哈尔滨工业大学 | A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics |
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| CN109942292A (en) * | 2019-04-12 | 2019-06-28 | 中南大学 | A kind of bismuth-sodium titanate base transparent ceramic material and its preparation method and application |
| CN109942292B (en) * | 2019-04-12 | 2021-09-07 | 中南大学 | Sodium bismuth titanate-based transparent ceramic material and preparation method and application thereof |
| CN114133239A (en) * | 2021-10-29 | 2022-03-04 | 湖北大学 | Lead-free pyroelectric ceramic material and preparation method thereof |
| CN114133239B (en) * | 2021-10-29 | 2022-09-06 | 湖北大学 | Lead-free pyroelectric ceramic material and preparation method thereof |
Also Published As
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| CN104961455B (en) | 2017-03-29 |
| CN104402432A (en) | 2015-03-11 |
| CN104947193A (en) | 2015-09-30 |
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