CN105036736A - Sodium-bismuth-titanate-base lead-free electrostrictive ceramic material and preparation method thereof - Google Patents
Sodium-bismuth-titanate-base lead-free electrostrictive ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a sodium-bismuth-titanate-base lead-free electrostrictive ceramic material and a preparation method thereof. The general formula of the material is (1-x)(Na0.5Bi0.5)TiO3-xSrTiO3-0.01KNbO3-ySm2O3-zY2O3, wherein x=0.45-0.60, y=0.01-0.02, and z=0.01-0.04. The preparation technique adopts a solid-phase process and comprises the following steps: respectively presintering and synthesizing (Na0.5Bi0.5)TiO3, SrTiO3 and KNbO3 powders, carrying out ball milling in an ethanol medium according to the stoichiometric proportion by using rare-earth Sm2O3 and Y2O3 as dopants to obtain a slurry, drying, grinding, carrying out extrusion forming, and sintering to obtain the ceramic. The ceramic material prepared by the method has favorable dispersivity when the dielectric peak is 20-50 DEG C, and the dispersion coefficient gamma is greater than 1.9. The ceramic material has favorable electrostrictive properties, and the maximum electrostriction value in a 40kv/cm electric field is 0.3%. The dielectric constant at room temperature under the condition of 1kHz is greater than 3500, and the dielectric loss is lower than 0.02. The material has the advantages of simple preparation technique and low price, is free of the harmful element Pb, satisfies the requirements for the environment-friendly material, and has favorable application prospects in the fields of ultrasonic transducers, micro shifters and the like.
Description
Technical field
The present invention relates to electrostriction ceramics technical field, particularly relate to a kind of bismuth-sodium titanate base lead-free electrostriction ceramics material and preparation method thereof.
Background technology
Electrostriction is a kind of basic electromechanical Coupling, and it is present among all solid matters.In early days because electrostrictive effect is general less, be not easily observed, even if strength of electric field reaches breaking down field strength, the field-induced strain of medium is also 10
-8the order of magnitude, compares to piezoelectric effect and magnetostrictive effect (10
-6) much smaller, so study seldom in simple solid matter.
Compared with piezoelectric effect, electrostriction material have do not need polarization, reproducible, without the advantage such as aging, so have important application prospect in fields such as micrometric displacement device, transverters.Current discovery in the relaxation ferroelectric of some high-ks, electrostrictive effect significantly and can be applied in application, and when temperature be in that it is ferroelectric-paraelectric phase transition areas adjacent time, electrostrictive effect has maximum value.The maximum of current application are leaded relaxation ferroelectrics, typical in lead zinc niobate-lead titanate (PZN-PT), the solid solution crystals of the class complex perovskite structure that PMN-PT (PMN-PT) is representative, they can cause lead volatility because of high sintering temperature.Therefore, developing no-lead electrostrictive material is the most important research topic in materialogy field.
Common unleaded relaxor ferroelectric crystal has potassium-sodium niobate-based (KNN), bismuth-sodium titanate (BNT) base Pb-Based Relaxor Ferroelectric Materials.Wherein KNN based leadless piezoelectric ceramics, due to the high (T of its Curie temperature
c=420 DEG C), low, the piezoelectric constant of specific inductivity and the characteristic such as electromechanical coupling factor is high, be considered to the piezoelectric of a kind of very promising replacement PZT, but due to the sintering characteristic of its difference, and easily there is deliquescence in a humid environment, limit the application [1] of such material.
CN201210251531 patent proposes a kind of Lead-free electrostrictive ceramic material and preparation method thereof, it is combined at potassium-sodium niobate-based (KNN) and bismuth-sodium titanate (BNT), and its Electrostrictive strain level under 70kV/cm electric field is ~ 0.137%.
CN201210336994 patent proposes unleaded ferroelectric/electrostrictive ceramic material, and it is combined at bismuth-sodium titanate (BNT) and bismuth titanates strontium, and its Electrostrictive strain level under 80kV/cm electric field is ~ 0.1%.
Mu Wenfang etc. [2] report (Bi
0.5na
0.5) TiO
3-BaTiO
3-SrTiO
3(BNT-BT-ST) pottery has higher disperse degree near accurate homotype phase boundary.Zhao [3] reports in BNT-ST system to find in ST molar content to be that 0.26 place exists accurate homotype phase boundary, all has certain relaxation property in ST molar content in 0 to 0.3 scope.
Reference:
[1]L.Egerton，D.M.Dillon，Piezoelectricanddielectricpropertiesofceramicsinthesystempotassium-sodiumniobateJ.Am.Ceram.Soc.1959,42:438-442.
[2] dielectric of Mu Wenfang, Du Huiling, Shi Xiang, Du Shaoming, BNT-BT-ST series lead-free piezoelectric ceramic material and ferroelectric properties [J]. silicate journal .2011,39:12
[3]ZhaoXL,YangWZ,LiuXQ,ChenXM.Dielectricandferroelectriccharacteristicsof[(Bi
0.5Na
0.5)
0.94Ba
0.06]
1-xSr
xTiO
3ceramics.JournalofMaterialsScience:MaterialsinElectronics.2014；25:1517-26.
Patents:
[1] CN200910021571 large-strain electrostriction ceramic material and preparation method thereof;
[2] CN201210240525 mono-kind bismuth-sodium titanate base lead-free pottery with high electrostriction coefficient and preparation method thereof;
[3] CN201210251531 Lead-free electrostrictive ceramic material and preparation method thereof;
[4] ferroelectric/electrostrictive ceramic material that CN201210336994 is unleaded.
Summary of the invention
The object of the present invention is to provide a kind of novel, unleaded, electrostriction material that dependent variable is large, solve the pollution problem existed in existing lead base electrostriction material production process, and develop its application in transverter and micrometric displacement device.
The present invention realizes like this.The present invention proposes a kind of no-lead electrostrictive material, and its chemical constitution formula is (1-x) (Na
0.5bi
0.5) TiO
3-xSrTiO
3-0.01KNbO
3-ySm
2o
3-zY
2o
3x=0.45 ~ 0.60 in formula, y=0.01 ~ 0.02, z=0.01 ~ 0.04; X, y, z represent SrTiO respectively
3, Sm
2o
3, Y
2o
3relative to principal constituent (1-x) (Na
0.5bi
0.5) TiO
3-xSrTiO
3mol ratio.
The present invention adopts Solid phase synthesis, and raw material is analytical pure NaCO
3, K
2cO
3, Bi
2o
3, TiO
2, SrCO
3, Sm
2o
3, Nb
2o
5and Y
2o
3.
Preparation method of the present invention is:
1. by analytical pure raw material NaCO
3, Bi
2o
3, TiO
2according to (Na
0.5bi
0.5) TiO
3stoichiometric ratio weighs, and carry out mixing and ball milling, ball-milling medium is ethanol, and rotating speed is 350 ~ 400r/min, and Ball-milling Time is 8 ~ 10h.
The slurry that ball milling is good washes out, and is placed in 100 DEG C of drying in oven, compacting of milling, and is placed in retort furnace and is at the uniform velocity warming up to 800 ~ 900 DEG C, and temperature rise rate is 3 DEG C/min, and insulation 2 ~ 8h, is cooled to room temperature in stove, mills and obtain powder A.
2. by analytical pure raw material SrCO
3, TiO
2according to SrTiO
3stoichiometric ratio weigh, carry out mixing and ball milling, ball-milling medium is ethanol, and rotating speed is 350 ~ 400r/min, and Ball-milling Time is 8 ~ 10h.
The slurry that ball milling is good washes out, and is placed in 100 DEG C of drying in oven, compacting of milling, and is placed in retort furnace and is at the uniform velocity warming up to 1150 ~ 1200 DEG C, and temperature rise rate is 3 DEG C/min, and insulation 2 ~ 8h, is cooled to room temperature in stove, mills and obtain powder B.
3. by analytical pure raw material K
2cO
3, Nb
2o
5according to KNbO
3stoichiometric ratio weigh, carry out mixing and ball milling, ball-milling medium is ethanol, and rotating speed is 350 ~ 400r/min, and Ball-milling Time is 8 ~ 10h.
The slurry that ball milling is good washes out, and is placed in 100 DEG C of drying in oven, compacting of milling, and is placed in retort furnace and is at the uniform velocity warming up to 750 ~ 850 DEG C, and temperature rise rate is 3 DEG C/min, and insulation 2 ~ 8h, is cooled to room temperature in stove, mills and obtain powder C.
4. by powder A, B, C, Sm
2o
3and Y
2o
3obtain slurry by stoichiometric ratio ball milling in ethanol medium of synthesis general formula, be placed in 80 ~ 100 DEG C of baking ovens and dry, mill, obtain powder D; Wherein x=0.45 ~ 0.60, y=0.01 ~ 0.02, z=0.01 ~ 0.04.
5. add in powder D massfraction be total powder quality 3 ~ 5%, mass concentration be 5% polyvinyl alcohol solution granulation, then make at 8 ~ 10Mpa pressure that diameter is 10 ~ 12mm, thickness is the sequin of 0.8 ~ 1mm, in 600 ~ 650 DEG C of binder removal 6 ~ 8h, gained disk is at 1180 ~ 1220 DEG C of sintering 2 ~ 4h, be cooled to room temperature in stove, namely obtain Low fire ceramic.
6. pair sample carries out surface treatment, and with 2000 order sand paper polishings, cleaning, after oven dry, evenly brush organic silver slurry, at 800 ~ 830 DEG C of silver ink firings, the time is 10 ~ 15 minutes.The ceramic print obtained containing electrode is cooled afterwards in stove.
Electrostriction material of the present invention at room temperature has cubic structure; There is good directric relaxation performance at dielectric peak in 20 ~ 50 DEG C of temperature ranges, and dispersion coefficient γ is greater than 1.9; Under room temperature 1kHz, specific inductivity is greater than 3500, and dielectric loss is lower than 0.02; Ferroelectric hysteresis loop is elongated, and under 40kv/cm electric field, maximum strain amount is 0.3%.
Principle of the present invention is such.We find in an experiment (1-x) Bi
0.5na
0.5tiO
3-x (SrTiO
3) ST molar content, in the scope of 0.45 to 0.60, can realize large room temperature relaxation property by rare earth doped in system, thus realize in large room temperature electrostrictive effect.Room temperature electrostriction of the present invention has been issued to 0.3% at 40KV/cm electric field, with lead-containing materials suitable (see patent CN200910021571), can realize substituting lead-containing materials.
Accompanying drawing explanation
Fig. 1 is the XRD of embodiment 1 sample;
Fig. 2 is the relation of specific inductivity and temperature under embodiment 1 sample different frequency;
Fig. 3 is the relation of dielectric loss and temperature under embodiment 1 sample different frequency;
Fig. 4 is the dispersivity exponent gamma figure of embodiment 1 sample;
Fig. 5 is ferroelectric hysteresis loop and the electrostriction curve of embodiment 1;
Embodiment
Specific embodiment 1:
1. by analytical pure raw material NaCO
3, Bi
2o
3, TiO
2according to (Na
0.5bi
0.5) TiO
3stoichiometric ratio weighs, and carry out mixing and ball milling, ball-milling medium is ethanol, and rotating speed is 400r/min, and Ball-milling Time is 10h.
2. washed out by the slurry that ball milling in step 1 is good, be placed in 100 DEG C of drying in oven, compacting of milling, be placed in retort furnace and be at the uniform velocity warming up to 800 DEG C, temperature rise rate is 3 DEG C/min, and insulation 2h, is cooled to room temperature in stove, mills and obtain powder A.
3. by analytical pure raw material SrCO
3, TiO
2according to SrTiO
3stoichiometric ratio weigh, carry out mixing and ball milling, ball-milling medium is ethanol, and rotating speed is 400r/min, and Ball-milling Time is 10h.
4. washed out by the slurry that ball milling in step 3 is good, be placed in 100 DEG C of drying in oven, compacting of milling, be placed in retort furnace and be at the uniform velocity warming up to 1150 DEG C, temperature rise rate is 3 DEG C/min, and insulation 2h, is cooled to room temperature in stove, mills and obtain powder B.
5. by analytical pure raw material K
2cO
3, Nb
2o
5according to KNbO
3stoichiometric ratio weigh, carry out mixing and ball milling, ball-milling medium is ethanol, and rotating speed is 400r/min, and Ball-milling Time is 10h.
6. washed out by the slurry that ball milling in step 5 is good, be placed in 100 DEG C of drying in oven, compacting of milling, be placed in retort furnace and be at the uniform velocity warming up to 750 DEG C, temperature rise rate is 3 DEG C/min, and insulation 2h, is cooled to room temperature in stove, mills and obtain powder C.
7. by powder A, powder B, powder C, Sm
2o
3and Y
2o
3carry out mixing and ball milling according to mol ratio 0.5:0.5:0.01:0.01:0.02, ball-milling medium is ethanol, and rotating speed is 350r/min, and Ball-milling Time is 8h.Slurry washes out the drying in oven being placed on 100 DEG C, mills and obtains powder D.
8. add in powder D massfraction be total powder quality 3%, mass concentration be 5% polyvinyl alcohol solution granulation, then make at 10Mpa pressure that diameter is 12mm, thickness is the sequin of 1mm, in 650 DEG C of binder removal 6h, gained disk is at 1200 DEG C of sintering 2h, and sintering heat-up rate is room temperature to 900 DEG C (3 DEG C/min), 900 to 1200 DEG C (2 DEG C/min); Be cooled to room temperature in stove, namely obtain Low fire ceramic.
9. pair ceramics sample carries out surface treatment, and with 2000 order sand paper polishings, cleaning, after oven dry, evenly brush organic silver slurry, at 830 DEG C of silver ink firings, the time is 10 minutes.The ceramics sample obtained containing electrode is cooled in stove.
10. the XRD of sample 1 as shown in Figure 1, and sample presents single cubic structure, meets the requirement preparing electrostriction material; Under different frequency, dielectric temperature relation as shown in Figure 2, and sample has larger specific inductivity, and under room temperature 1kHz, specific inductivity is 3827; Under different frequency, loss temperature relation as shown in Figure 3, and sample has lower dielectric loss, and under room temperature 1kHz, loss is lower than 0.02; As shown in Figure 4, sample has good frequency dispersal in the change of dispersivity exponent gamma, and disperse exponent gamma is 1.94; As shown in Figure 5, sample ferroelectric hysteresis loop is elongated for ferroelectric hysteresis loop, and remnant polarization and coercive field are all less; As shown in Figure 5, this material has good electrostrictive property in electrostriction, and under 40kv/cm electric field, maximum strain amount is 0.3%.
Claims (4)
1. a bismuth-sodium titanate base lead-free electrostriction ceramics material, is characterized in that synthesis general formula is: (1-x) (Na
0.5bi
0.5) TiO
3-xSrTiO
3-0.01KNbO
3-ySm
2o
3-zY
2o
3x=0.45 ~ 0.60 in formula, y=0.01 ~ 0.02, z=0.01 ~ 0.04; X, y, z represent SrTiO respectively
3, Sm
2o
3, Y
2o
3relative to principal constituent (1-x) (Na
0.5bi
0.5) TiO
3-xSrTiO
3mol ratio.
2. a preparation method for bismuth-sodium titanate base lead-free electrostriction ceramics material, is characterized in that preparation technology in turn includes the following steps:
1). by analytical pure raw material NaCO
3, Bi
2o
3, TiO
2according to (Na
0.5bi
0.5) TiO
3stoichiometric ratio weighs, and carry out mixing and ball milling, ball-milling medium is ethanol, rotating speed is 350 ~ 400r/min, Ball-milling Time is 8 ~ 10h, and the slurry that ball milling is good washes out, and is placed in 100 DEG C of drying in oven, to mill compacting, be placed in retort furnace and be at the uniform velocity warming up to 800 ~ 900 DEG C, temperature rise rate is 3 DEG C/min, insulation 2 ~ 8h, be cooled to room temperature in stove, mill and obtain powder A;
2). by analytical pure raw material SrCO
3, TiO
2according to SrTiO
3stoichiometric ratio weigh, carry out mixing and ball milling, ball-milling medium is ethanol, rotating speed is 350 ~ 400r/min, Ball-milling Time is 8 ~ 10h, and the slurry that ball milling is good washes out, and is placed in 100 DEG C of drying in oven, to mill compacting, be placed in retort furnace and be at the uniform velocity warming up to 1150 ~ 1200 DEG C, temperature rise rate is 3 DEG C/min, insulation 2 ~ 8h, be cooled to room temperature in stove, mill and obtain powder B;
3). by analytical pure raw material K
2cO
3, Nb
2o
5according to KNbO
3stoichiometric ratio weigh, carry out mixing and ball milling, ball-milling medium is ethanol, rotating speed is 350 ~ 400r/min, Ball-milling Time is 8 ~ 10h, and the slurry that ball milling is good washes out, and is placed in 100 DEG C of drying in oven, to mill compacting, be placed in retort furnace and be at the uniform velocity warming up to 750 ~ 850 DEG C, temperature rise rate is 3 DEG C/min, insulation 2 ~ 8h, be cooled to room temperature in stove, mill and obtain powder C;
4). by powder A, B, C, Sm
2o
3and Y
2o
3obtain slurry by stoichiometric ratio ball milling in ethanol medium of synthesis general formula, be placed in 80 ~ 100 DEG C of baking ovens and dry, mill, obtain powder D; Wherein x=0.45 ~ 0.60, y=0.01 ~ 0.02, z=0.01 ~ 0.04;
5). add in powder D massfraction be total powder quality 3 ~ 5%, mass concentration be 5% polyvinyl alcohol solution granulation, then make at 8 ~ 10MPa pressure that diameter is 10 ~ 12mm, thickness is the sequin of 0.8 ~ 1mm, in 600 ~ 650 DEG C of binder removal 6 ~ 8h, gained disk is at 1180 ~ 1220 DEG C of sintering 2 ~ 4h, be cooled to room temperature in stove, namely obtain Low fire ceramic;
6). ceramic plate is carried out surface treatment to sample, silver electrode in burning, obtain ceramic product of the present invention.
3. the preparation method of a kind of bismuth-sodium titanate base lead-free electrostriction ceramics material according to claim 2, is characterized in that in preparation technology the 4th step, x=0.5, y=0.01, z=0.02.
4. the preparation method of a kind of bismuth-sodium titanate base lead-free electrostriction ceramics material according to claim 2, is characterized in that in preparation technology the 6th step, sintering buries burning with zirconia powder.
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Cited By (4)
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| CN107253857A (en) * | 2017-06-26 | 2017-10-17 | 陕西科技大学 | A kind of unleaded high energy storage density ceramic material and preparation method thereof |
| CN107344851A (en) * | 2017-06-26 | 2017-11-14 | 陕西科技大学 | A kind of wide temperature area temperature stabilizing type ceramic capacitor material of bismuth-sodium titanate base lead-free and preparation method thereof |
| CN111875389A (en) * | 2020-08-13 | 2020-11-03 | 西安科技大学 | Method for regulating and controlling performance of lead-free piezoelectric ceramic |
| CN113511893A (en) * | 2021-03-24 | 2021-10-19 | 广西大学 | BNT-based high-energy-density ceramic with three-layer structure and preparation method thereof |
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| CN107344851A (en) * | 2017-06-26 | 2017-11-14 | 陕西科技大学 | A kind of wide temperature area temperature stabilizing type ceramic capacitor material of bismuth-sodium titanate base lead-free and preparation method thereof |
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| CN113511893A (en) * | 2021-03-24 | 2021-10-19 | 广西大学 | BNT-based high-energy-density ceramic with three-layer structure and preparation method thereof |
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