CN103224389A - Lead-free electrostrictive ceramic based on barium titanate, and preparation method thereof - Google Patents
Lead-free electrostrictive ceramic based on barium titanate, and preparation method thereof Download PDFInfo
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- CN103224389A CN103224389A CN2013101381519A CN201310138151A CN103224389A CN 103224389 A CN103224389 A CN 103224389A CN 2013101381519 A CN2013101381519 A CN 2013101381519A CN 201310138151 A CN201310138151 A CN 201310138151A CN 103224389 A CN103224389 A CN 103224389A
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Abstract
The invention discloses a lead-free electrostrictive ceramic based on barium titanate, and a preparation method thereof. Raw material components and molar ratio percentage content thereof are 50Ba(Zr0.35Ti0.65)O3-50(Ba0.75Ca0.25)TiO3, and on the basis, 1-7wt% of CaO-Al2O3-SiO2 (referred to CAS) is added. A conventional solid-phase synthesis preparation method is employed to obtain the lead-free electrostrictive ceramic with relatively low sintering temperature, relaxation characteristics and a large electrostrictive coefficient. The lead-free electrostrictive ceramic is simple in components and process steps. The preparation method is convenient for operation, has good repeatability and high yield. The lead-free electrostrictive ceramic is mainly applied to energy converters, micro actuators, etc.
Description
Technical field
The invention relates to the composition is the ceramic composition of feature, relates in particular to a kind of at 0.5Ba (Zr
0.35Ti
0.65) O
3-0.5 (Ca
0.25Ba
0.75) TiO
3The basis on add CaO-Al
2O
3-SiO
2(CAS) barium titanate-based lead-free electrostriction ceramics and preparation method thereof.
Background technology
The strain that is directly proportional with the field intensity quadratic power that dielectric medium produced under External Electrical Field is called electrostriction.This effect caused by polarization of dielectric in the electric field, and can occur in all dielectric mediums, it is characterized in that strained positive and negative with the external electric field orientation independent.In piezoelectrics, external electric field can also cause the strain of another kind of type, and its size is proportional with field intensity, when the outer positive and negative also opposite sign of strain when field-reversed.The latter is the adverse affects of piezoelectric effect, is not electrostriction.The overall strain of the caused piezoelectrics of external electric field is inverse piezoelectric effect and electrostrictive effect sum.For non-piezoelectrics, external electric field only causes the electrostriction strain.Usually, the little several magnitude of inverse piezoelectric effect of the caused strain ratio piezoelectrics of electrostriction.To in common dielectric, obtain to be equivalent to piezoelectrics the strain of getable size, external electric field needs up to 10
8V/m.But in the very high dielectric medium of some specific inductivity, even external electric field is lower than 10
6V/m also can obtain the mechanical electric coupling close with strong piezoelectrics and provides technology to use.Electrostrictive another characteristics are that its circulation ratio is better in application.Strengthen outside under the direct current biasing electric field action, for synergetic alternating electric field, the ferroelectricity piezoelectric ceramics commonly used that the hysteresis of the electromechanical Coupling of electrostriction material and catabiosis compare is much smaller.This advantage makes electrostrictive effect be usually used in aspects such as pressure survey, continuous tunable laser, bistable state photoelectric device.
Present most electrostriction material is the material of plumbiferous relaxation ferroelectric composite perofskite type structure, as lead magnoniobate, lead zinc niobate etc.And relaxation ferroelectric ceramic has very high specific inductivity, big electrostrictive effect, low relatively sintering temperature and cause low temperature coefficient of capacitance by disperse phase transformation (Diffuse Phase Transition is called for short DPT), and it is the excellent material of making micro positioner.Because lead has toxicity, and environment and human body are had harm, so the plumbous use of restriction in the world now.But because electrostriction material has become indispensable material in modern high-tech field, so we must seek its substitute, no-lead electrostrictive material more and more is subject to people's attention like this.
Along with the hyundai electronics fast development of information technology, exploitation and exploration for the excellent performance dielectric substance have become the hot issue that various countries are studied, at present, mainly adopt 2 kinds of methods aspect improvement in performance: a kind of is doping vario-property, and certain modification ion promptly mixes; Another kind is to improve preparation technology, with BaTiO
3(BT) be matrix, obtain 0.5Ba (Zr by mixing and changing preparation technology
0.35Ti
0.65) O
3-0.5 (Ca
0.25Ba
0.75) TiO
3Electrostriction material, this dielectric material has high specific inductivity, electric field adjustability and Curie temperature adjustability and advantage such as leaded environmental sound not because of it, in the no-lead electrostrictive material development, has very large prospect, but the sintering temperature higher (1300 ℃ or more) of this material in preparation, so just caused the waste on the cost, therefore guaranteeing to obtain preferably on the dielectric properties and big strained basis, we take suitably to adjust prescription and form the sintering temperature that reduces material.
Summary of the invention
Purpose of the present invention is to solve 0.5Ba (Zr
0.35Ti
0.65) O
3-0.5 (Ca
0.25Ba
0.75) TiO
3The too high drawback of bringing of system electrostriction ceramics sintering temperature adds CaO-Al
2O
3-SiO
2(eutectoid point is 1170 ℃) three-part system reduces sintering temperature, a kind of energy lower temperature sintering is provided and can guarantees that it has the 0.5Ba (Zr of better electrostrictive property
0.35Ti
0.65) O
3-0.5 (Ca
0.25Ba
0.75) TiO
3The system electrostriction ceramics.
The present invention is achieved by the following technical programs:
A kind of barium titanate-based lead-free electrostriction ceramics, feed composition and mole percent level thereof are 50Ba (Zr
0.35Ti
0.65) O
3-50 (Ba
0.75Ca
0.25) TiO
3, add the CaO-Al of 1～7wt% on this basis
2O
3-SiO
2, be called for short CAS;
This barium titanate-based lead-free electrostriction ceramics gets the preparation method, and preparation process is as follows:
(1) batching is synthetic
Press 50Ba (Zr
0.35Ti
0.65) O
3-50 (Ba
0.75Ca
0.25) TiO
3Stoichiometric ratio take by weighing former BaCO
3, CaCO
3, ZrO
2And TiO
2Mix, in the ball grinder of packing into, ball-milling medium is water and agate ball, ball: material: the weight ratio of water is 2: 1: 0.6, and ball milling 4h, rotational speed of ball-mill are 750 rev/mins, compound is put into 80 ℃ of oven dry of baking oven again, puts into mortar again and grinds, and crosses 80 mesh sieves;
(2) pre-burning
Powder after grinding in the step (1), sieving is put into crucible,, add a cover sealing with the compacting of agate rod; Carry out pre-burning in 1150 ℃ in retort furnace, insulation 2h naturally cools to room temperature, comes out of the stove;
(3) secondary ball milling
Adding massfraction in step (2) in the powder of oven dry is that the adding massfraction is 1～7% CaCO
3, Al
2O
3And SiO
2, CaCO
3, Al
2O
3And SiO
2Consist of 23.3%:14.7%:62.0%, powder is ground in mortar, cross 80 mesh sieves, the ball grinder of packing into, ball: material: the weight ratio of water is 2: 1: 0.6, secondary ball milling 6h again, rotating speed 750rad/min puts into 80 ℃ of oven dry of baking oven with powder;
(4) granulation
Powder porphyrize in mortar with step (3) oven dry sieves, and the adding weight percent is 5%～10% polyvinyl alcohol, fully stirs, and sieves, and powder is put into the stainless steel mould that diameter is 35 ㎜, depresses to cylindric blank at 100-120Mpa pressure;
(5) moulding
Powder in the step (4) after the granulation leaves standstill 24h, powder is put into the stainless steel mould that diameter is 15 ㎜ again, depresses to cylindric blank at 300Mpa pressure;
(6) binder removal
Blank in the step (5) is put into retort furnace,, temperature rises to 400 ℃, and insulation 1h carries out organism and gets rid of;
(7) sintering
Blank behind the binder removal in the step (6) is put into crucible, seal, do to bury with similar powder and expect to bury burning, sintering in 1250 ℃, insulation 2h naturally cools to room temperature with stove;
(8) burn electrode
With the ceramic plate that sinters in the step (7) polish to thickness be 0.6 ㎜, dry naturally, lower surface applies the silver slurry thereon, places stove to be warming up to 735 ℃, insulation 10min naturally cools to room temperature;
(9) dielectric properties of test article and electrostrictive property.
Described no-lead electrostrictive pottery is single perovskite structure.
Described no-lead electrostrictive pottery is 6 ℃/minute in the heat-up rate of step (7).
The preparation method of described no-lead electrostrictive pottery adopts traditional solid phase synthesis process.
Described no-lead electrostrictive pottery has improved relaxation behavior.
Described no-lead electrostrictive pottery has big electrostriction coefficient.
The invention has the beneficial effects as follows that sintering has gone out a kind of have bigger electrostriction coefficient, good barium phthalate base (BT) the no-lead electrostrictive pottery of over-all properties under the lower sintering temperature.The present invention adopts the method for traditional solid phase synthesis, and (BT) is matrix with barium titanate, and with Zr, Ca is that doping agent has obtained barium calcium zirconate titanate (BCZT), adds CaO-Al on this basis
2O
3-SiO
2The three component system sintering agent, it is lower to have obtained a kind of sintering temperature, has the no-lead electrostrictive pottery of obvious improved relaxation behavior and big electrostriction coefficient.Composition of the present invention and processing step are simple, easy handling, good reproducibility, yield rate height.
Description of drawings
Fig. 1 is the surface topography map of the BCZT system sample of the embodiment of the invention 1,2,3,4;
Fig. 2 is the ferroelectric hysteresis loop of the BCZT system sample of the embodiment of the invention 1,2,3,4;
Fig. 3 is BCZT system electric field-strain curve (S of the embodiment of the invention 1,2,3,4
33-E);
Fig. 4 is the strain S of the BCZT system of the embodiment of the invention 1,2,3,4
33With polarizability square (P
2) curve spectrum.
Embodiment
The present invention adopts commercially available chemical pure raw material (purity 〉=99%), is BaCO
3, CaCO
3, ZrO
2, TiO
2, Al
2O
3And SiO
2
Barium titanate-based lead-free electrostriction ceramics of the present invention, its feed composition and mole percent level 50Ba (Zr thereof
0.35Ti
0.65) O
3-50 (Ba
0.75Ca
0.25) TiO
3, add the CaO-Al of 1～7wt% on this basis
2O
3-SiO
2, be called for short CAS;
The present invention adopts the method for traditional solid phase synthesis, and concrete preparation process is:
(1) batching is synthetic
Press 50Ba (Zr
0.35Ti
0.65) O
3-50 (Ba
0.75Ca
0.25) TiO
3Stoichiometric ratio take by weighing former BaCO
3, CaCO
3, ZrO
2And TiO
2Mix, in the ball grinder of packing into, ball-milling medium is water and agate ball, ball: material: the weight ratio of water is 2: 1: 0.6, and ball milling 4h, rotational speed of ball-mill are 750 rev/mins, compound is put into 80 ℃ of oven dry of baking oven again, puts into mortar again and grinds, and crosses 80 mesh sieves;
(2) pre-burning
Powder after step (1) ground, sieves is put into crucible, with the compacting of agate rod, adds a cover sealing; Give burning in 1150 ℃ in retort furnace, insulation 2h naturally cools to room temperature, comes out of the stove;
(3) secondary ball milling
The adding massfraction is 1～7% CaCO in the powder of drying in step (2)
3, Al
2O
3And SiO
2, CaCO
3, Al
2O
3And SiO
2Consist of 23.3%:14.7%:62.0%, in mortar, grind, cross 80 mesh sieves, the ball grinder of packing into, ball: material: the weight ratio of water is 2: 1: 0.6, secondary ball milling 6h again, rotating speed 750rad/min puts into 80 ℃ of oven dry of baking oven with powder;
(4) granulation
Powder porphyrize in mortar with step (3) oven dry sieves, and the adding weight percent is 5%～10% polyvinyl alcohol (PVA), fully stir, sieve, powder is put into the stainless steel mould that diameter is 35 ㎜, depress to cylindric blank at 100-120Mpa pressure.
(5) moulding
Powder after the granulation in the step (4) is left standstill 24h, again powder is put into the stainless steel mould that diameter is 15 ㎜, depress to cylindric blank at 300Mpa pressure;
(6) binder removal
Blank in the step (5) is put into retort furnace, and temperature rises to 400 ℃, and insulation 1h carries out organism and gets rid of;
(7) sintering
Blank behind the binder removal in the step 6) is put into crucible, seal, do to bury with similar powder and expect to bury burning, heat-up rate is 6 ℃/minute, sintering in 1250 ℃, and insulation 2h naturally cools to room temperature with stove;
(8) burn electrode
With the ceramic plate that sinters in the step (7) polish to thickness be 0.6 ㎜, dry naturally, lower surface applies the silver slurry thereon, places 735 ℃ of insulations of stove 10min, naturally cools to room temperature;
(9) dielectric properties of test article and electrostrictive property.
Specific embodiment is as follows:
X=1, sintering temperature is 1250 ℃, is designated as embodiment 1;
X=3, sintering temperature is 1250 ℃, is designated as embodiment 2;
X=5, sintering temperature is 1250 ℃, is designated as embodiment 3;
X=7, sintering temperature is 1250 ℃, is designated as embodiment 4;
The electrostrictive property test result of the foregoing description is listed in table 1.
Means of testing is: the axial electric field induced strain with DGS-6A type digital display type inductance amesdial measurement sample axially applies voltage with DC high-voltage power supply along sample.Electrostriction coefficient Q
33Try to achieve according to following formula:
Q
33＝S
33/P
2
Wherein: S
33Be electric field induced strain, P is a polarizability.
Table 1
As can see from Figure 1, after sintering temperature was 1250 ℃, its tissue topography had obtained tangible improvement, grain growth and pattern very clear.Density is also thereupon the improve of sintering temperature and increase.Along with the increase of sintering agent, we see that the glassy phase at crystal boundary place also increases thereupon gradually, but also cause the reduction of ceramic dielectric performance simultaneously.
See that from Fig. 2 along with the variation ferroelectric hysteresis loop of AS content has clearly difference, when AS content was 1wt% and 3wt%, the area that loop line surrounded was very big, remnant polarization and coercive field are also very big.And when AS content be 5%wt when above, loop line obviously reduces, it is very little that remnant polarization and coercive field also become.The adding that AS is described is to 0.5Ba (Zr
0.35Ti
0.65) O
3-0.5 (Ca
0.25Ba
0.75) TiO
3The ferroelectricity influence of pottery is very big, and along with the increase of AS content, its ferroelectricity weakens.
As shown in Figure 3, AS content is that their pairing maximum strains of 1wt%, 3wt%, 5wt% and 7wt% are respectively 0.042%, 0.055%, 0.064% and 0.055%.Can see that the maximum strain amount has elder generation to increase the trend that afterwards reduces with the increase of AS content.This be because under the low situation of AS content pottery at low temperatures during sintering its density not high enough, have very most of strain to be absorbed by pore.Along with the increase of AS content, density increases, and when reaching 7wt%, glassy phase is more in the pottery, and it is very little even can not produce strain to the strained contribution amount, so strain reduces.
Fig. 4 is 0.5Ba (Zr
0.35Ti
0.65) O3-0.5 (Ca
0.25Ba
0.75) TiO
3Pottery its strain polarizability curve (S when 1250 ℃ of sintering
33-P
2) with AS content curve.The power taking field orientation is the curve linear match of forward when boosting, according to formula S
33=Q
33P
2Obtain electrostriction coefficient Q value.Calculate Q
33Along with the increase of AS content is respectively 0.027m
4C
-2, 0.063m
4C
-2, 0.142m
4C
-2And 0.263m
4C
-2, that is to say that the increase electrostriction coefficient along with AS content increases, be exactly S so show from figure
33-P
2Curve is steeper, promptly just can reach bigger strain under less polarizability.Figure goes up and shows that linear relationship was good more when AS content was higher in addition, particularly when polarizability is big.
Claims (6)
1. barium titanate-based lead-free electrostriction ceramics, feed composition and mole percent level thereof are 50Ba (Zr
0.35Ti
0.65) O
3-50 (Ba
0.75Ca
0.25) TiO
3, add the CaO-Al of 1～7wt% on this basis
2O
3-SiO
2, be called for short CAS;
This barium titanate-based lead-free electrostriction ceramics gets the preparation method, and preparation process is as follows:
(1) batching is synthetic
Press 50Ba (Zr
0.35Ti
0.65) O
3-50 (Ba
0.75Ca
0.25) TiO
3Stoichiometric ratio take by weighing former BaCO
3, CaCO
3, ZrO
2And TiO
2Mix, in the ball grinder of packing into, ball-milling medium is water and agate ball, ball: material: the weight ratio of water is 2: 1: 0.6, and ball milling 4h, rotational speed of ball-mill are 750 rev/mins, compound is put into 80 ℃ of oven dry of baking oven again, puts into mortar again and grinds, and crosses 80 mesh sieves;
(2) pre-burning
Powder after grinding in the step (1), sieving is put into crucible,, add a cover sealing with the compacting of agate rod; Carry out pre-burning in 1150 ℃ in retort furnace, insulation 2h naturally cools to room temperature, comes out of the stove;
(3) secondary ball milling
Adding massfraction in step (2) in the powder of oven dry is that the adding massfraction is 1～7% CaCO
3, Al
2O
3And SiO
2, CaCO
3, Al
2O
3And SiO
2Consist of 23.3%:14.7%:62.0%, powder is ground in mortar, cross 80 mesh sieves, the ball grinder of packing into, ball: material: the weight ratio of water is 2: 1: 0.6, secondary ball milling 6h again, rotating speed 750rad/min puts into 80 ℃ of oven dry of baking oven with powder;
(4) granulation
Powder porphyrize in mortar with step (3) oven dry sieves, and the adding weight percent is 5%～10% polyvinyl alcohol, fully stirs, and sieves, and powder is put into the stainless steel mould that diameter is 35 ㎜, depresses to cylindric blank at 100-120Mpa pressure;
(5) moulding
Powder in the step (4) after the granulation leaves standstill 24h, powder is put into the stainless steel mould that diameter is 15 ㎜ again, depresses to cylindric blank at 300Mpa pressure;
(6) binder removal
Blank in the step (5) is put into retort furnace,, temperature rises to 400 ℃, and insulation 1h carries out organism and gets rid of;
(7) sintering
Blank behind the binder removal in the step (6) is put into crucible, seal, do to bury with similar powder and expect to bury burning, sintering in 1250 ℃, insulation 2h naturally cools to room temperature with stove;
(8) burn electrode
With the ceramic plate that sinters in the step (7) polish to thickness be 0.6 ㎜, dry naturally, lower surface applies the silver slurry thereon, places stove to be warming up to 735 ℃, insulation 10min naturally cools to room temperature;
(9) dielectric properties of test article and electrostrictive property.
2. according to the barium titanate-based lead-free electrostriction ceramics of claim 1, it is characterized in that described no-lead electrostrictive pottery is single perovskite structure.
3. according to the barium titanate-based lead-free electrostriction ceramics of claim 1, it is characterized in that described no-lead electrostrictive pottery is 6 ℃/minute in the heat-up rate of step (7).
4. according to the barium titanate-based lead-free electrostriction ceramics of claim 1, it is characterized in that the preparation method of described no-lead electrostrictive pottery adopts traditional solid phase synthesis process.
5. according to the barium titanate-based lead-free electrostriction ceramics of claim 1, it is characterized in that described no-lead electrostrictive pottery has improved relaxation behavior.
6. according to the barium titanate-based lead-free electrostriction ceramics of claim 1, it is characterized in that described no-lead electrostrictive pottery has big electrostriction coefficient.
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| CN1410390A (en) * | 2001-09-27 | 2003-04-16 | 株式会社村田制作所 | Dielectric ceramic composition and capacitor using same |
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| CN102815938A (en) * | 2012-08-27 | 2012-12-12 | 天津大学 | Barium titanate-based lead-free electrostrictive ceramics and preparation method thereof |
-
2013
- 2013-04-19 CN CN2013101381519A patent/CN103224389A/en active Pending
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|---|---|---|---|---|
| CN1410390A (en) * | 2001-09-27 | 2003-04-16 | 株式会社村田制作所 | Dielectric ceramic composition and capacitor using same |
| CN1382662A (en) * | 2002-02-20 | 2002-12-04 | 中国科学院上海硅酸盐研究所 | Low-temp sinter process for squar-phase zirconium oxide polycrystal with stabilized nano yttrium oxide |
| CN1477081A (en) * | 2003-07-11 | 2004-02-25 | 清华大学 | High-toughness Al2O3/Ti3SiC2 laminate ceramic composite material and its hot-pressing preparation method |
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Application publication date: 20130731 |