CN1715242A - Bismuth-sodium titanate-bismuth potassium titanate barium zirconate titanate lead free piezoelectric ceramics - Google Patents
Bismuth-sodium titanate-bismuth potassium titanate barium zirconate titanate lead free piezoelectric ceramics Download PDFInfo
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- CN1715242A CN1715242A CN 200510085014 CN200510085014A CN1715242A CN 1715242 A CN1715242 A CN 1715242A CN 200510085014 CN200510085014 CN 200510085014 CN 200510085014 A CN200510085014 A CN 200510085014A CN 1715242 A CN1715242 A CN 1715242A
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Abstract
The present invention discloses a kind of environment friendly lead-free bismuth sodium titanate-bismuth potassium tatanate-barium zirconate titanate piezoelectric ceramic in functional ceramic preparing technology. The lead-free piezoelectric ceramic has the general expression of (1-x)Bi1/2(Na1-zKz)1/2TiO3-xBa(ZryTi1-y)O3, where, x is BZT molar content, y is atom number of Zr to replace Ti in BaTiO3, z is atom number of K to replace Na in BaNaO3, x is 0-0.1, y is 0-0.10 and z is 0-0.05. The lead-free piezoelectric ceramic may be prepared with industrial materials and through traditional piezoelectric ceramic preparing technological process. The lead-free piezoelectric ceramic has d33 up to 16pC/N, Curie temperature up to 270 deg c and practical application value.
Description
Technical field
The invention belongs to the function ceramics preparing technical field.Be particularly related to the bismuth-sodium titanate-bismuth potassium titanate barium zirconate titanate leadless piezoelectric ceramics of a class calcium attitude ore deposit structural environment Harmony.
Background technology
Piezoelectric ceramics is that a class is important, and the hi tech and new material that international competition is very fierce is widely used in high-tech sectors such as information, laser, navigation and biologies, but the extensive now piezoelectric ceramics that uses mainly is the lead base piezoelectric ceramics, i.e. PbTiO
3-PbZrO
3, PbT
iO
3-PbZrO
3-ABO
3(ABO
3Be the composite perofskite type ferroelectrics) and PbTiO
3Series piezoelectric ceramic etc.(or the Pb of PbO in these stupaliths
3O
4) content account for about 70%.The lead base piezoelectric produce, use and discarded last handling process in bring serious harm all can for the mankind and ecotope, this and human social are disagreed.Therefore researching and developing leadless piezoelectric material material is a problem that great society and economic implications are arranged.
Leadless piezoelectric ceramics, or title environment compatibility piezoelectric ceramics, be meant the new functional type stupalith of a class that not only has satisfied use properties but also have good environment compatibility, it requires material system itself not contain the hurtful material of ecotope possibility (particularly plumbous), and not producing in preparation, use, waste treatment process may deleterious material to environment, and preparation technology should have power consumption less, good environment compatibility such as environmental pollution is little.The leadless piezoelectric ceramics system that can be considered up to now, has: BaTiO
3Based leadless piezoelectric ceramics; Bi
1/2Na
1/2TiO
3(BNT) based leadless piezoelectric ceramics; Niobate lead-free piezoelectric ceramics; Bismuth laminated leadless piezoelectric ceramic.
In recent years, occurred numerous ceramic systems in the leadless piezoelectric ceramics, but compared, very big gap had still been arranged on the performance, therefore also needed a large amount of research-and-development activitys with the lead base piezoelectric ceramics with practical prospect.Design angle from material, existing lead-free systems is done the theoretical investigation of further doping vario-property and the replacement of B position, A position, understand fully the chemical property that replaces atom to ceramic micro-structure and Effect on Performance, significant for the high performance leadless piezoelectric ceramics system of exploitation.In addition, research and development is different from the new ceramics processing of traditional ceramics technology of preparing, makes the microtexture of pottery present certain single crystal feature, is another important development direction of leadless piezoelectric ceramics research.
Bismuth-sodium titanate (Bi
1/2Na
1/2) TiO
3(BNT) be the composite perofskite ferroelectrics of nineteen sixty by people such as Smolensky invention, belong to trigonal system during room temperature, Curie temperature is 320 ℃.BNT has strong (the room temperature remnant polarization P of ferroelectricity
r=38C/cm
2), piezo-electric modulus is big, and specific inductivity is little, and acoustical behavior waits good characteristic well, and sintering temperature is low, is considered to one of the most attractive lead-free piezoceramic material system.Yet, the coercive field height (E of BNT
c=73kV/cm),, thereby be difficult to polarization at the specific conductivity height of ferroelectric phase region.Na in addition
2The easy moisture absorption of O, the sintering range of pottery is narrow, causes the stable chemical performance of system relatively poor.Along with the reduction of temperature, it has two phase transition processes: by cube being transformed into cubic phase mutually, 230 ℃ become oblique side's phase by tetragonal phase converting in the time of 520 ℃.And the transition process from the four directions to oblique side, pottery becomes ferroelectric state by antiferroelectric state, shows very peculiar dielectric properties.In addition, because its conductivity height, the leakage conductance electric current is big, makes very difficult that its polarization becomes.Therefore must mix or introduce other element and structure on this basis.
In recent years, people have carried out a large amount of study on the modification to the BNT base piezoelectric ceramic.Research is thought, BNT based leadless piezoelectric ceramics A position compound ion (Bi
1/2Na
1/2)
2+Ion is Bi especially
3+Ion is that this is the strong major cause of ceramic ferroelectricity.A position Bi
3+Content the ferroelectric piezoelectric properties such as Curie temperature, electromechanical coupling factor, mechanical quality factor, remnant polarization and coercive field strength of pottery are had great effect.Research and development to the BNT based leadless piezoelectric ceramics at present mainly concentrate on A, the B position, the particularly substituting modification of A position.For example: patent CN85100426, JP11-217262, JP2000-22235, JP2000-272962 provide ABO
3The composition formula of structure is [Bi
0.5(Na
1-xK
x)
0.5] TiO
3The piezoelectric ceramics compound, its A position is Bi, Na, K; The B position is Ti.For example: patent CN85100426, JP11-217262, JP2000-22235, JP2000-272962 provide ABO
3The composition formula of structure is [Bi
0.5(Na
1-xK
x)
0.5] TiO
3The piezoelectric ceramics compound, its A position is Bi, Na, K; The B position is Ti.It is (1-x) Bi that patent CN 200410088425.9 has also provided composition formula
1/2Na
1/2TiO
3-xBa (Zr
yTi
1-y) O
3The piezoelectric ceramics compound, its A position is Bi, Na; The B position is Ti, Zr.But preparation and the performance about BNT-BKT-BZT ternary system leadless piezoelectric ceramics yet there are no report at present.
Summary of the invention
Purpose of the present invention is exactly in order to overcome the inherent defective of existing lead base piezoelectric ceramics system own, has proposed the bismuth-sodium titanate-bismuth potassium titanate barium zirconate titanate leadless piezoelectric ceramics of ternary system.It is characterized in that: the bismuth-sodium titanate-bismuth potassium titanate barium zirconate titanate leadless piezoelectric ceramics of described ternary system is with general formula (1-x) Bi
1/2(Na
1-zK
z)
1/2TiO
3-xBa (Zr
yTi
1-y) O
3Expression, wherein x is the molar content of BZT in the ceramic systems, y is BaTiO
3In the Ti atom by Zr metathetical atomicity, z is BiNaO
3In the Na atom by K metathetical atomicity; 0＜x≤0.1,0＜y≤0.10,0＜z≤0.05.
Its preparation technology is according to 0.9 ((1-z) Bi
1/2Na
1/2TiO
3-zBi
1/2K
1/2TiO
3)-0.1Ba (Zr
yTi
1-y) O
3Theoretical content carry out proportioning, with Na
2CO
3, Bi
2O
3, BaCO
3, K
2CO
3, TiO
2, ZrO
2Powder is, with the dehydrated alcohol is the ball-milling medium ball milling, be pressed into disk after 70 ℃ of dryings, insulation was synthesized in 2 hours under 800～950 ℃ of temperature, 200 orders that sieve, the acid polyethylene PVA solution of 3wt% concentration that adds 0.5～1.5ml according to every 10g compound is pressed into diameter 10mm as binding agent under 150MPa pressure, the disk of thickness 1～1.5mm is incubated 3 hours down at 1100～1200 ℃.Sample after burning till polishes and by silver electrode, with the condition polarization of 4kV/mm, removes electric field after 20 minutes polarization times in the silicone oil of the sample behind the silver ink firing under 80 ℃, takes out sample.
The calcium attitude ore deposit type leadless piezoelectric ceramics that the present invention proposes has good piezoelectricity ferro performance.In its material property parameter, piezoelectric constant d
33Can reach more than the 165pC/N, Curie temperature reaches 270 ℃.Advantage of the present invention is: 1, material system is a leadless piezoelectric ceramics; 2, piezoelectricity ferro excellent property; 3, process stabilizing; 4, can adopt conventional piezoelectric ceramics processing and industrial starting material to obtain, have the value of practical application.
Description of drawings
Fig. 1 is 1150 ℃ of sintering BNKT-BZT ceramic surface SEM figure.
Fig. 2 is that (y=0.04, z=0.020), (b) (y=0.45, BNKT-BZT ceramics sample different frequency z=0.025) be Jie's temperature spectrum down for s23 for (a) s11.
Embodiment
With reference to MPB (accurate homotype phase boundary) the position 0.900BNT-0.10BZT of BNT-BZT, according to 0.9 ((1-z) Bi
1/2Na
1/2TiO
3-zBi
1/2K
1/2TiO
3)-0.1Ba (Zr
yTi
1-y) O
3Theoretical content carry out proportioning, adopt analytically pure raw material, use Na
2CO
3, Bi
2O
3, BaCO
3, K
2CO
3, TiO
2, ZrO
2Powder is a raw material powder, the design mix proportioning is as shown in table 1, after the weighing, be the ball-milling medium ball milling accurately, be pressed into disk after 70 ℃ of dryings with the dehydrated alcohol, insulation was synthesized in 2 hours under 800～950 ℃ of temperature, 200 orders that sieve, the PVA solution of 3wt% concentration that adds 0.5～1ml according to every 10g compound is pressed into diameter 10mm as binding agent under 150MPa pressure, the disk of thickness 1～1.5mm is incubated 3 hours down at 1150 ℃.Sample after burning till polishes and by silver electrode, with the condition polarization of 4kV/mm, removes electric field after 20 minutes polarization times in the silicone oil of the sample behind the silver ink firing under 80 ℃, takes out sample.At last, by the IRE standard piezoelectric ceramics of making is measured performance perameters such as piezoelectricity.
Embodiment
According to 0.9 ((1-z) Bi
1/2Na
1/2TiO
3-zBi
1/2K
1/2TiO
3)-0.1Ba (Zr
yTi
1-y) O
3Theoretical content carry out proportioning, with reference to the MPB position of BNT-BKT, adopt Na
2CO
3, Bi
2O
3, BaCO
3, K
2CO
3, TiO
2And ZrO
2Analytically pure powder stock, according to forming shown in the table 1, specifically by after respectively organizing the accurate weighing of weight shown in the table 3, grouping is the ball-milling medium ball milling with the dehydrated alcohol, is pressed into disk after 70 ℃ of dryings, insulation was synthesized in 2 hours under 800～950 ℃ of temperature, 200 orders that sieve, the PVA solution of 3wt% concentration that adds 0.5～1.5ml according to every 10g compound is pressed into diameter 10mm as binding agent under 150MPa pressure, the disk of thickness 1～1.5mm is incubated 3h down at 1150 ℃.Sample after burning till polishes and by silver electrode, with the condition polarization of 4kV/mm, removes electric field after 20 minutes polarization times in the silicone oil of the sample behind the silver ink firing under 80 ℃, takes out sample.At last, by the IRE standard piezoelectric ceramics of making is measured performance perameters such as piezoelectricity.
Each component sample of table 1
| Sample | Sample is formed |
| s11 | 0.9Bi 1/2(Na 0.98 K 0.02) 1/2TiO 3-0.1Ba(Zr 0.04Ti 0.96)O 3 |
| s12 | 0.9Bi 1/2(Na 0.97 K 0.03) 1/2TiO 3-0.1Ba(Zr 0.04Ti 0.96)O 3 |
| s21 | 0.9Bi 1/2(Na 0.98 K 0.02) 1/2TiO 3-0.1Ba(Zr 0.045Ti 0.955)O 3 |
| s22 | 0.9Bi 1/2(Na 0.975 K 0.025) 1/2TiO 3-0.1Ba(Zr 0.045Ti 0.955)O 3 |
| s23 | 0.9Bi 1/2(Na 0.97 K 0.03) 1/2TiO 3-0.1Ba(Zr 0.045Ti 0.955)O 3 |
| s24 | 0.9Bi 1/2(Na 0.965 K 0.035) 1/2TiO 3-0.1Ba(Zr 0.045Ti 0.955)O 3 |
| s31 | 0.9Bi 1/2(Na 0.97 K 0.03) 1/2TiO 3-0.1Ba(Zr 0.05Ti 0.95)O 3 |
| s32 | 0.9Bi 1/2(Na 0.965 K 0.035) 1/2TiO 3-0.1Ba(Zr 0.04Ti 0.96)O 3 |
Each component sample electric property of table 2.
| Piezoelectric constant sample title d 33(pC/N) | Loss tg | Planar electromechanical coupling factor K p | Mechanical quality factor Q m | ||
| s11 s12 s21 s22 s23 s24 s31 s32 | 162 160 145 165 153 141 153 152 | 1210.112 1127.662 706.1686 562.8383 743.6609 669.2396 1046.099 998.3655 | 0.0396 0.0384 0.0396 0.0334 0.0387 0.0388 0.0346 0.0342 | 0.168065 0.170406 0.185404 0.179044 0.170722 0.222491 0.136769 0.166742 | 31.55017 35.25438 30.15686 37.59694 28.77708 68.12298 27.99868 27.72108 |
Table 3 BNKT-BZT ceramics component proportioning
| The sample title | Y | z | Bi 2O 3 (g) | Na 2CO 3(g) | BaCO 3 (g) | TiO 2(g) | ZrO 2(g) | K 2CO 3 (g) |
| s11 s12 s21 s22 s23 s24 s31 s32 | 0.04 0.04 5 0.05 | 0.02 0.03 0.02 0.025 0.03 0.035 0.03 0.035 | 5.24211 | 1.16853 1.15660 1.16853 1.16257 1.15660 1.15064 1.15660 1.15064 | 0.98668 | 3.97732 3.99129 3.97332 | 0.02465 0.02773 0.03081 | 0.03110 0.04664 0.03110 0.03887 0.04664 0.05442 0.04664 0.05442 |
1, SEM experimental analysis: Fig. 1 is the typical pattern (s31) of ceramic crystalline grain, and crystal grain is piled up closely, does not have tangible gross blow hole, and the void content of sample is low, densified sintering product.The ceramic crystalline grain size is in 2～5um scope.
2, Curie temperature test: the Curie temperature of having tested sample s11 and s23.As can be seen from Figure 2, the Curie temperature of two samples is all about 270 ℃.
3, piezoelectric property and dielectric properties test: as can be seen from Table 2, be about 2.5% at K content, Zr content is 4.5% d of place
33Value reach 165.And at Zr content is 4% d of place
33Value also reach 160.Dielectric constant values is in 600～1200 scopes.
Claims (2)
1. bismuth-sodium titanate-bismuth potassium titanate barium zirconate titanate leadless piezoelectric ceramics, it is characterized in that: the bismuth-sodium titanate-bismuth potassium titanate barium zirconate titanate leadless piezoelectric ceramics of described ternary system is with general formula (1-x) Bi
1/2(Na
1-zK
z)
1/2TiO
3-xBa (Zr
yTi
1-y) O
3Expression, wherein x is the molar content of BZT in the ceramic systems, y is BaTiO
3In the Ti atom by Zr metathetical atomicity, z is BiNaO
3In the Na atom by K metathetical atomicity; 0＜x≤0.1,0＜y≤0.10,0＜z≤0.05.
2. the preparation technology of the described bismuth-sodium titanate-bismuth potassium titanate barium zirconate titanate leadless piezoelectric ceramics of claim 1, it is characterized in that: its preparation technology is as follows:
According to 0.9 ((1-z) Bi
1/2Na
1/2TiO
3-zBi
1/2K
1/2TiO
3)-0.1Ba (Zr
yTi
1-y) O
3Theoretical content carry out proportioning, with Na
2CO
3, Bi
2O
3, BaCO
3, K
2CO
3, TiO
2, ZrO
2Powder is a raw material, with the dehydrated alcohol is the ball-milling medium ball milling, mix, be pressed into disk after 70 ℃ of dryings, insulation was synthesized in 2 hours under 800～950 ℃ of temperature, and 200 orders sieve, the acid polyethylene PVA solution of 3wt% concentration that adds 0.5～1.5ml according to every 10g compound is as binding agent, be pressed into diameter 10mm under 150MPa pressure, the disk of thickness 1～1.5mm is incubated 3 hours down at 1100～1200 ℃; Sample after burning till polishes and by silver electrode, with the condition polarization of 4kV/mm, removes electric field after 20 minutes polarization times in the silicone oil of the sample behind the silver ink firing under 80 ℃, takes out sample.
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| CN101973763A (en) * | 2010-09-16 | 2011-02-16 | 合肥工业大学 | Potassium-bismuth titanate-based solid solution lead-free piezoelectric ceramic and manufacturing method thereof |
| CN102199035A (en) * | 2011-03-22 | 2011-09-28 | 清华大学 | X9r ceramic capacitor dielectric material and preparation method thereof |
| CN101767992B (en) * | 2010-01-14 | 2012-05-09 | 哈尔滨理工大学 | Sol-gel method for preparing Zr(BiNa)BaTiO lead-free piezoelectric ceramic nano powder |
| CN104230332A (en) * | 2013-06-14 | 2014-12-24 | 佛山市南海金刚新材料有限公司 | Printing nozzle piezoelectric element and preparation method thereof |
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| CN111592350A (en) * | 2020-06-04 | 2020-08-28 | 西安工业大学 | BKT-based energy storage dielectric material with temperature stability and synthesis method thereof |
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| JP4437848B2 (en) * | 1999-03-24 | 2010-03-24 | Ｎｅｃトーキン株式会社 | Piezoelectric ceramic composition |
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| CN101767992B (en) * | 2010-01-14 | 2012-05-09 | 哈尔滨理工大学 | Sol-gel method for preparing Zr(BiNa)BaTiO lead-free piezoelectric ceramic nano powder |
| CN101973763A (en) * | 2010-09-16 | 2011-02-16 | 合肥工业大学 | Potassium-bismuth titanate-based solid solution lead-free piezoelectric ceramic and manufacturing method thereof |
| CN101973763B (en) * | 2010-09-16 | 2013-01-02 | 合肥工业大学 | Potassium-bismuth titanate-based solid solution lead-free piezoelectric ceramic and manufacturing method thereof |
| CN102199035A (en) * | 2011-03-22 | 2011-09-28 | 清华大学 | X9r ceramic capacitor dielectric material and preparation method thereof |
| CN102199035B (en) * | 2011-03-22 | 2013-06-26 | 清华大学 | X9r ceramic capacitor dielectric material and preparation method thereof |
| CN104230332A (en) * | 2013-06-14 | 2014-12-24 | 佛山市南海金刚新材料有限公司 | Printing nozzle piezoelectric element and preparation method thereof |
| US10056539B2 (en) | 2014-04-30 | 2018-08-21 | Oregon State University | Electrocaloric device |
| CN111592350A (en) * | 2020-06-04 | 2020-08-28 | 西安工业大学 | BKT-based energy storage dielectric material with temperature stability and synthesis method thereof |
| CN114315350A (en) * | 2022-01-24 | 2022-04-12 | 武汉理工大学 | Sodium bismuth titanate-barium zirconate titanate lead-free wide-temperature energy storage ceramic and preparation method thereof |
| CN114315350B (en) * | 2022-01-24 | 2023-05-23 | 武汉理工大学 | Bismuth sodium titanate-barium zirconate titanate leadless wide-temperature energy storage ceramic and preparation method thereof |
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