CN101962292A - Alkali metal niobium-tantalum antimonite-based leadless piezoelectric ceramic and preparation method thereof - Google Patents

Alkali metal niobium-tantalum antimonite-based leadless piezoelectric ceramic and preparation method thereof Download PDF

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CN101962292A
CN101962292A CN 201010286524 CN201010286524A CN101962292A CN 101962292 A CN101962292 A CN 101962292A CN 201010286524 CN201010286524 CN 201010286524 CN 201010286524 A CN201010286524 A CN 201010286524A CN 101962292 A CN101962292 A CN 101962292A
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piezoelectric ceramic
tantalum
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metal niobium
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左如忠
付健
刘义
苏石
齐世顺
赵万里
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Hefei University of Technology
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Abstract

The invention discloses alkali metal niobium-tantalum antimonite-based leadless piezoelectric ceramic modified by barium-based cubic perovskite and a preparation method thereof. The alkali metal niobium-tantalum antimonite-based leadless piezoelectric ceramic is indicated by a general formula of (1-u) [(NaxKy) (Nbx+y-zSbz)O3+(1-x-y-v)LiTaO3+vBaMeO3]+uM. The alkali metal niobium-tantalum antimonite-based leadless piezoelectric ceramic has a morphotropic phase boundary of a rhombic ferroelectric phase and a square ferroelectric phase as well as good sintering property and piezoelectric property, is good-performance leadless series environmental harmony piezoelectric ceramic, can replace the traditional partial leady piezoelectric ceramic and can be obtained by adopting the traditional piezoelectric ceramic preparation technology and industrial materials and has practicability.

Description

Basic metal niobium tantalum stibnate based leadless piezoelectric ceramics and preparation method
Technical field
The present invention relates to leadless piezoelectric ceramics and preparation method thereof, specifically basic metal niobium tantalum stibnate based leadless piezoelectric ceramics and preparation method thereof.
Background technology
Since over half a century, with Pb-based lanthanumdoped zirconate titanates (Pb (Zr, Ti) O 3, PZT) for the piezoelectric ceramics of main component has been widely used in electronics, space flight, communication, numerous areas such as military affairs.Such as, piezoelectric ceramics is made various wave filters, vibrator, electronic components such as wavetrap.Yet the content of plumbous oxide or tri-lead tetroxide accounts for more than 70% in these piezoceramic materials.Bring serious harm all can in the treating processes of these plumbiferous piezoelectric ceramics after using and discarding human beings'health and living environment.
Bismuth-sodium titanate is the ferroelectric ceramic(s) of a kind of research unleaded type with perovskite structure early, wherein the accurate homotype phase boundary of bismuth-sodium titanate and barium titanate formation is formed, have good piezoelectricity and electromechanical coupling performance (T.Takenaka, K.Maruyama, and K.Sakata, Jpn.J.Appl.Phys., 30 (1991) 2236; CA1456531A, CN1511800A, CN1673178, JP1999-329533, JP2000-272962).Yet the polarization field intensity is higher, and the umpolarization temperature is lower, and piezoelectric property is on the low side, has limited its practical application.
In recent years, base metal niobate mainly is to have potassium niobate that accurate homotype phase boundary forms to receive (Na 0.5K 0.5NbO 3, be called for short NKN) noted widely.Yet this pottery is difficult in sintering under the conventional preparation technology, and is easy to hydrolysis, thereby its electrical property is not in full use.By Li, after an amount of doping of Ta or Sb, its sintering process and piezoelectric property are improved (Y.Saito, H.Takao, I.Tani, T.Nonoyama, K.Takatori, T.Homma, T.Nagaya, Nature, 432 (2004) 84) greatly.
Yet the basic metal niobium tantalum stibnate based leadless piezoelectric ceramics of bibliographical information all is based on the composition of quadrature ferroelectric phase and cubic ferroelectric phase phase boundary at present, is different from the lead piezoelectric ceramics that contains of traditional PZT base.It all is the phase boundary that is positioned at rhombus ferroelectric phase and cubic ferroelectric phase that these traditional lead base piezoelectric ceramics are formed.Barium base cubic perovskite is formed the effect with stable rhombus phase, be expected to help the base metal niobate compositional system to form the phase boundary that is similar to the conventional piezoelectric pottery, but yet there are no the electrical property of basic metal niobium tantalum stibnate based leadless piezoelectric ceramics of cubic perovskite modification of barium base and preparation technology's research report in the existing document.
Summary of the invention
The invention provides basic metal niobium tantalum stibnate based leadless piezoelectric ceramics of a kind of barium base cubic perovskite modification and preparation method thereof for overcoming the deficiencies in the prior art.The pottery composition of this system has the accurate homotype phase boundary of rhombus ferroelectric phase and cubic ferroelectric phase, and good sintering property and piezoelectric property.
The technical scheme that technical solution problem of the present invention is adopted is:
Basic metal niobium tantalum stibnate based leadless piezoelectric ceramics, its spy is characterised in that: it is formed component and is expressed by following general formula:
(1-u)[(Na xK y)(Nb x+y-zSb z)O 3+(1-x-y-v)LiTaO 3+vBaMeO 3]+uM (1)
X in the formula, y, z, u, v are each element shared atomic percent in material component, and value is all less than 1;
And: x 〉=0.52, y 〉=0.4,0＜z≤0.08,1-x-y-v＞0, v＞0 and 0＜u＜0.02;
M eBe selected from Zr 4+, Hf 4+, Sn 4+In the quaternary metal ion one or more;
M is selected from the oxide compound of Na, K, Li, Ag, Cu, Fe, Mn, Zn, Nd, Sm, Yb, Sc metal or the carbonate one or more.
The preparation method of described basic metal niobium tantalum stibnate based leadless piezoelectric ceramics is characterized in that: may further comprise the steps:
A, with Na 2CO 3, K 2CO 3, Li 2CO 3, Nb 2O 5, Ta 2O 5, Sb 2O 5, ZrO 2, HfO 2, SnO 2, and be used for adulterated metal oxide or carbonate is raw material, prepare burden according to formula (1);
B, confected materials are medium with the dehydrated alcohol, behind 6-12 hour ball mill mixing, drying obtains dry powder; Gained dry powder temperature with 850-1050 ℃ in alumina crucible was calcined 1-4 hour; Repeat ball mill mixing and calcining process once, it is synthetic to finish precalcining;
C, pre-synthetic powder still are medium fine grinding 22-26 hour again with the dehydrated alcohol after grinding, and dried powder crosses that the forming under the pressure at 50-200MPa is a base substrate behind the 110-130 mesh sieve;
Base substrate after d, the moulding adopts under the normal pressure in air and buries the powder method sintering, and places two crucibles of putting upside down, and sintering temperature is 1000-1250 ℃, and sintering time is that 1-4 hour, temperature rise rate are 1.5-2.5 ℃/min;
E, burn till product through after the polished finish by silver electrode, back making alive in silicone oil polarizes, polarizing voltage is 1.5-3.5kV/mm, the polarization temperature is 25-150 ℃, the polarization time is 5-30 minute;
F, make the test that the piezoelectric ceramics sample carries out piezoelectricity and electromechanical coupling performance according to the standard of IRE.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, pottery of the present invention is formed the piezoelectric ceramics of the environment compatibility that is a kind of well behaved unleaded system, can realize substituting to the plumbiferous conventional piezoelectric pottery of part, and its stable preparation process can adopt the technology of preparing of conventional piezoelectric pottery and industrial raw material to obtain, and has practicality.
2, the present invention can obtain to have the pottery composition of rhombus ferroelectric phase and the accurate homotype phase boundary of cubic ferroelectric phase structure by the relative content of adjusting barium base cubic perovskite and lithium tantalum antimony, thereby reaches excellent piezoelectricity and electromechanical coupling performance.
3, leadless piezoelectric ceramics of the present invention repeats batch mixing by twice and calcining process improves the composition homogeneity with complex component system; and adopt and to bury the volatilization loss that powder method and two crucible protection methods reduce potassium sodium lithium; thereby it is controlled to obtain a kind of stoichiometry, and the good leadless piezoelectric ceramics of piezoelectric property.
4, ceramic formula of the present invention effectively improves sintering densification behavior and the grain growth behavior that matrix is formed by the doping of the metal oxide of trace, as reduce sintering temperature, improve sintered density, suppress grain growth, thereby optimize various piezoelectricity and electromechanical coupling performance, satisfy the needs of different occasions.
Description of drawings
Fig. 1 consists of among the embodiment 1:
(1-u) [(Na 0.52K 0.4) (Nb 0.84Sb 0.08) O 3+ (0.08-v) LiTaO 3+ vBaZrO 3]+uCuO, and the sample when u=0.005 and v=0.025 is at the stereoscan photograph of 1150 ℃ of sintering after 2 hours.
Fig. 2 consists of among the embodiment 1:
(1-u) [(Na 0.52K 0.4) (Nb 0.84Sb 0.08) O 3+ (0.08-v) LiTaO 3+ vBaZrO 3]+uCuO, and the dielectric-temperature curve of sample when 100kHz when u=0.005 and v=0.025.
Fig. 3 consists of among the embodiment 1:
(1-u) [(Na 0.52K 0.4) (Nb 0.84Sb 0.08) O 3+ (0.08-v) LiTaO 3+ vBaZrO 3]+uCuO, and u=0.005, and v is respectively the X-ray diffractogram of 0.01,0.025,0.04 o'clock sample.
Fig. 4 consists of among the embodiment 1:
(1-u) [(Na 0.52K 0.4) (Nb 0.84Sb 0.08) O 3+ (0.08-v) LiTaO 3+ vBaZrO 3]+uCuO, and u=0.005, and v is respectively the ferroelectric hysteresis loop of 0.01,0.025,0.04 o'clock sample when 1150 ℃ of sintering.
Fig. 5 consists of among the embodiment 1:
(1-u) [(Na 0.53K 0.42) (Nb 0.89Sb 0.06) O 3+ (0.05-v) LiTaO 3+ vBaHfO 3]+uAgO, and the sample when u=0.005 and v=0.015 is at the stereoscan photograph of 1180 ℃ of sintering after 2 hours.
Fig. 6 consists of among the embodiment 1:
(1-u) [(Na 0.52K 0.42) (Nb 0.87Sb 0.07) O 3+ (0.06-v) LiTaO 3+ vBaSnO 3]+uMnO 2, and the X-ray diffractogram under differing temps of sample when u=0.005 and v=0.02.
Embodiment
In concrete the enforcement, the component that the basic metal niobium tantalum stibnate based leadless piezoelectric ceramics of barium base cubic perovskite modification is expressed by following general formula is formed:
(1-u)[(Na xK y)(Nb x+y-zSb z)O 3+(1-x-y-v)LiTaO 3+vBaMeO 3]+uM (1)
X in the formula, y, z, u, v are each element shared atomic percent in material component,
And: x 〉=0.52, y 〉=0.4,0＜z≤0.08,1-x-y-v＞0, v＞0 and 0＜u＜0.02;
M eBe selected from Zr 4+, Hf 4+, Sn 4+In the quaternary metal ion one or more;
M is selected from the oxide compound of Na, K, Li, Ag, Cu, Fe, Mn, Zn, Nd, Sm, Yb, Sc metal or the carbonate one or more.
The preparation method of the basic metal niobium tantalum stibnate based leadless piezoelectric ceramics of above-mentioned barium base cubic perovskite modification is:
With technical pure or chemical pure anhydrous sodium carbonate (Na 2CO 3), Anhydrous potassium carbonate (K 2CO 3), Quilonum Retard (Li 2CO 3), Niobium Pentxoxide (Nb 2O 5), tantalum pentoxide (Ta 2O 5), antimony peroxide (Sb 2O 5), barium titanate (BaCO 3), zirconium dioxide (ZrO 2), hafnium oxide (HfO 2), tindioxide (SnO 2) and be used for adulterated metal oxide and carbonate is raw material, prepare burden according to the composition of general formula (1), finish pre-synthetic through ball mill mixing and calcining successively; Pre-synthetic powder is a base substrate through fine grinding and high-pressure molding; Sintering under the normal pressure; Burning till product polarization handles.
Preparation method's concrete steps are:
1, with Na 2CO 3, K 2CO 3, Li 2CO 3, Nb 2O 5, Ta 2O 5, Sb 2O 5, ZrO 2, HfO 2, SnO 2, and be used for adulterated metal oxide and carbonate is raw material, prepare burden according to formula (1);
2, confected materials is medium with the dehydrated alcohol, behind 6-12 hour ball mill mixing, drying obtains dry powder; Gained dry powder temperature with 850-1050 ℃ in alumina crucible was calcined 1-4 hour; Repeat ball mill mixing and calcining process once, it is synthetic to finish precalcining;
3, pre-synthetic powder is through after grinding still with the dehydrated alcohol being medium fine grinding 24 hours again, and dried powder crosses that the forming under the pressure at 50-200MPa is a base substrate behind 120 mesh sieves;
4, the base substrate after the moulding adopts under the normal pressure in air and buries the powder method sintering, and to place the double crucible of putting upside down, sintering temperature be 1000-1250 ℃, and sintering time is that 1-4 hour, temperature rise rate are 2 ℃/min;
5, burn till product through after the polished finish by silver electrode, back making alive in silicone oil polarizes, polarizing voltage is 1.5-3.5kV/mm, the polarization temperature is 25-150 ℃, the polarization time is 5-30 minute;
6, make the test that the piezoelectric ceramics sample carries out piezoelectricity and electromechanical coupling performance according to the standard of IRE.
The present embodiment ceramic formula is by following general formula
(1-u) [(Na xK y) (Nb X+y-zSb z) O 3+ (1-x-y-v) LiTaO 3+ vBaMeO 3]+uM represents.
Embodiment 1
Carry out each step successively by above-mentioned embodiment, wherein,
Adopt (1-u) [(Na 0.52K 0.4) (Nb 0.84Sb 0.08) O 3+ (0.08-v) LiTaO 3+ vBaZrO 3The piezoelectric ceramics of]+uCuO for forming, precalcining temperature are that 900 ℃, time are 4 hours.It after twice calcining is ball-milling medium ball milling 24 hours once more with the dehydrated alcohol.And the base substrate of aftershaping sintering 2 hours in 1000-1250 ℃ scope.
U=0.005, the sample of v=0.025 at the stereoscan photograph of 1150 ℃ of sintering natural surface after 2 hours as shown in Figure 1, its dielectric-temperature characteristics such as Fig. 2.
Work as u=0.005, v=0.01, the X ray diffracting spectrum of 0.025 and 0.04 o'clock two composition sample is as shown in Figure 3.
Work as u=0.005, v=0.01 forms the ferroelectric hysteresis loop of sample behind 1150 ℃ of sintering as shown in Figure 4 for 0.025 and 0.04 o'clock two.
Work as u=0.005, v=0.025 and sintering temperature are 1150 ℃, and sintering time is 2 hours, record other physicals such as table 1 of sample:
Table 1
Embodiment 2
Carry out each step successively by above-mentioned embodiment, wherein
Adopt (1-u) [(Na 0.53K 0.42) (Nb 0.89Sb 0.06) O 3+ (0.05-v) LiTaO 3+ vBaHfO 3]+uAgO, and u=0.005, the piezoelectric ceramics of forming during v=0.015, the condition of precalcining is 950 ℃, the time is 3 hours.It after twice calcining is ball-milling medium ball milling 24 hours once more with the dehydrated alcohol.And the base substrate of aftershaping is 1180 ℃ of sintering 2 hours, the stereoscan photograph of its sample natural surface as shown in Figure 5, other relevant physical performance data is listed in table 2:
Table 2
Figure BSA00000276174300061
Embodiment 3
Carry out each step successively by above-mentioned embodiment, wherein,
Adopt (1-u) [(Na 0.52K 0.42) (Nb 0.87Sb 0.07) O 3+ (0.06-v) LiTaO 3+ vBaSnO 3]+uMnO 2, and u=0.005, the piezoelectric ceramics of forming during v=0.02, the condition of precalcining is 1000 ℃, is incubated 3 hours.It after twice calcining is ball-milling medium ball milling 24 hours once more with the dehydrated alcohol.And the base substrate of aftershaping is 1200 ℃ of sintering 2 hours, the X-ray diffractogram of its sample under differing temps as shown in Figure 6, other relevant performance data is listed in table 3:
Table 3
Figure BSA00000276174300062

Claims (2)

1. basic metal niobium tantalum stibnate based leadless piezoelectric ceramics is characterized in that: it is formed component and is expressed by following general formula:
(1-u)[(Na xK y)(Nb x+y-zSb z)O 3+(1-x-y-v)LiTaO 3+vBaMeO 3]+uM (1)
X in the formula, y, z, u, v are respectively each element shared atomic percent in material component, and value is all less than 1;
And: x 〉=0.52, y 〉=0.4,0＜z≤0.08,1-x-y-v＞0, v＞0 and 0＜u＜0.02;
M eBe selected from Zr 4+, Hf 4+, Sn 4+In the quaternary metal ion one or more;
M is selected from the oxide compound of Na, K, Li, Ag, Cu, Fe, Mn, Zn, Nd, Sm, Yb, Sc metal or the carbonate one or more.
2. the preparation method of basic metal niobium tantalum stibnate based leadless piezoelectric ceramics as claimed in claim 1 is characterized in that: may further comprise the steps:
A, with Na 2CO 3, K 2CO 3, Li 2CO 3, Nb 2O 5, Ta 2O 5, Sb 2O 5, ZrO 2, HfO 2, SnO 2, and be used for adulterated metal oxide or carbonate is raw material, prepare burden according to formula (1);
B, confected materials are medium with the dehydrated alcohol, behind 6-12 hour ball mill mixing, drying obtains dry powder; Gained dry powder temperature with 850-1050 ℃ in alumina crucible was calcined 1-4 hour; Repeat ball mill mixing and calcining process once, it is synthetic to finish precalcining;
C, pre-synthetic powder still are medium fine grinding 22-26 hour again with the dehydrated alcohol after grinding, and dried powder crosses that the forming under the pressure at 50-200MPa is a base substrate behind the 110-130 mesh sieve;
Base substrate after d, the moulding adopts under the normal pressure in air and buries the powder method sintering, and places two crucibles of putting upside down, and sintering temperature is 1000-1250 ℃, and sintering time is that 1-4 hour, temperature rise rate are 1.5-2.5 ℃/min;
E, burn till product through after the polished finish by silver electrode, back making alive in silicone oil polarizes, polarizing voltage is 1.5-3.5kV/mm, the polarization temperature is 25-150 ℃, the polarization time is 5-30 minute;
F, make the test that the piezoelectric ceramics sample carries out piezoelectricity and electromechanical coupling performance according to the standard of IRE.
CN 201010286524 2010-09-16 2010-09-16 Alkali metal niobium-tantalum antimonite-based leadless piezoelectric ceramic and preparation method thereof Expired - Fee Related CN101962292B (en)

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WO2015093436A1 (en) * 2013-12-16 2015-06-25 日立金属株式会社 Piezoelectric ceramic with crystal orientation, production method therefor, and piezoelectric element
CN108585851A (en) * 2018-07-10 2018-09-28 合肥工业大学 A kind of unleaded no potassium high-power piezoelectric ceramic of sodium niobate base and preparation method thereof
CN110668808A (en) * 2019-10-17 2020-01-10 新疆大学 SnO with high nonlinearity, low residual voltage and large through-current capacity for power transmission of power system2Piezoresistor and preparation method thereof
CN112062562A (en) * 2020-09-17 2020-12-11 广西大学 Preparation method of KNN-based ultrahigh breakdown electric field single crystal thin film material
CN112194464A (en) * 2020-10-28 2021-01-08 中科传感技术(青岛)研究院 Sintering method for lead-containing piezoelectric ceramic product
CN112341160A (en) * 2020-11-06 2021-02-09 南京工业大学 Broadband high-Q low-temperature coefficient barium-magnesium-calcium-niobium-tantalum composite ceramic and preparation method thereof
CN112510171A (en) * 2019-09-13 2021-03-16 株式会社东芝 Composite oxide, active material composite material, electrode, battery pack, and vehicle

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CN101311139A (en) * 2007-05-24 2008-11-26 西北工业大学 Leadless piezoelectric ceramics with bismuth ion replacing modified potassium sodium niobate base and method for preparing same
CN101343178A (en) * 2008-08-14 2009-01-14 广东风华高新科技股份有限公司 (ZrSnZnNb)TiO4 microwave ceramic dielectric material and preparation thereof

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WO2015093436A1 (en) * 2013-12-16 2015-06-25 日立金属株式会社 Piezoelectric ceramic with crystal orientation, production method therefor, and piezoelectric element
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CN112062562B (en) * 2020-09-17 2022-04-19 广西大学 Preparation method of KNN-based ultrahigh breakdown electric field single crystal thin film material
CN112194464A (en) * 2020-10-28 2021-01-08 中科传感技术(青岛)研究院 Sintering method for lead-containing piezoelectric ceramic product
CN112341160A (en) * 2020-11-06 2021-02-09 南京工业大学 Broadband high-Q low-temperature coefficient barium-magnesium-calcium-niobium-tantalum composite ceramic and preparation method thereof

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