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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 CN201010286524.3A CN201010286524A CN101962292A CN 101962292 A CN101962292 A CN 101962292A CN 201010286524 A CN201010286524 A CN 201010286524A CN 101962292 A CN101962292 A CN 101962292A
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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

本发明公开了一种钡基立方钙钛矿改性的碱金属铌钽锑酸盐基无铅压电陶瓷及其制备方法，以通式(1-u)[(NaxKy)(Nbx+y-zSbz)O3+(1-x-y-v)LiTaO3+vBaMeO3]+uM来表示。本发明的陶瓷组成具有菱形铁电相和四方铁电相的准同型相界，以及良好的烧结特性和压电性能，是一种性能良好的无铅系的环境协调性的压电陶瓷，可实现对部分含铅的传统压电陶瓷的替代，可采用传统压电陶瓷的制备技术和工业用原料获得，具有实用性。

Figure 201010286524

The invention discloses an alkali metal niobium tantalum antimonate-based lead-free piezoelectric ceramic modified by barium-based cubic perovskite and a preparation method thereof. The general formula (1-u)[(Na x K y )(Nb x+yz Sb z )O 3 +(1-xyv)LiTaO 3 +vBaMeO 3 ]+uM. The ceramic composition of the present invention has quasi-isomorphic phase boundaries of rhombic ferroelectric phase and tetragonal ferroelectric phase, and good sintering characteristics and piezoelectric properties. It is a lead-free piezoelectric ceramic with good performance and environmental coordination. Realize the replacement of part of the traditional piezoelectric ceramics containing lead, can be obtained by using the preparation technology of traditional piezoelectric ceramics and industrial raw materials, and has practicability.

Figure 201010286524

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.碱金属铌钽锑酸盐基无铅压电陶瓷，其特征在于：其组成组分由以下通式来表达：1. Alkali metal niobium tantalum antimonate-based lead-free piezoelectric ceramics, characterized in that: its components are expressed by the following general formula: (1-u)[(NaxKy)(Nbx+y-zSbz)O3+(1-x-y-v)LiTaO3+vBaMeO3]+uM  (1)(1-u)[(Na x K y )(Nb x+yz Sb z )O 3 +(1-xyv)LiTaO 3 +vBaMeO 3 ]+uM (1) 式中x，y，z，u，v分别为各元素在材料组分中所占的原子百分比，取值均小于1；In the formula, x, y, z, u, and v are the atomic percentages of each element in the material component, and the values are all less than 1; 并且：x≥0.52、y≥0.4、0＜z≤0.08、1-x-y-v＞0、v＞0以及0＜u＜0.02；And: x≥0.52, y≥0.4, 0<z≤0.08, 1-x-y-v>0, v>0 and 0<u<0.02; Me选自Zr4+、Hf4+、Sn4+四价的金属离子中的一种或多种；Me is selected from one or more of Zr 4+ , Hf 4+ , and Sn 4+ tetravalent metal ions; M选自Na、K、Li、Ag、Cu、Fe、Mn、Zn、Nd、Sm、Yb、Sc金属的氧化物或者碳酸盐中一种或多种。M is selected from one or more of Na, K, Li, Ag, Cu, Fe, Mn, Zn, Nd, Sm, Yb, Sc metal oxides or carbonates. 2.如权利要求1所述的碱金属铌钽锑酸盐基无铅压电陶瓷的制备方法，其特征在于：包括以下步骤：2. the preparation method of alkali metal niobium tantalum antimonate base lead-free piezoelectric ceramics as claimed in claim 1, is characterized in that: comprise the following steps: a、以Na2CO3，K2CO3，Li2CO3，Nb2O5，Ta2O5，Sb2O5，ZrO2，HfO2，SnO2，以及用于掺杂的金属氧化物或者碳酸盐为原料，按照式(1)配料；a. With Na 2 CO 3 , K 2 CO 3 , Li 2 CO 3 , Nb 2 O 5 , Ta 2 O 5 , Sb 2 O 5 , ZrO 2 , HfO 2 , SnO 2 , and metal oxides for doping Compound or carbonate is raw material, according to formula (1) batching; b、配好的原料以无水乙醇为介质，经6-12小时的球磨混料后、干燥得到干粉；所得干粉在氧化铝坩埚中以850-1050℃的温度煅烧1-4小时；重复球磨混料和煅烧工艺一次，完成预煅烧合成；b. The prepared raw materials use absolute ethanol as the medium, and after 6-12 hours of ball milling and mixing, dry to obtain dry powder; the obtained dry powder is calcined in an alumina crucible at a temperature of 850-1050°C for 1-4 hours; repeated ball milling The mixing and calcination process is done once to complete the pre-calcination synthesis; c、预合成的粉体经过研碎后仍以无水乙醇为介质再细磨22-26小时，干燥后的粉体过110-130目筛后在50-200MPa的压力下成型为坯体；c. After the pre-synthesized powder is ground, it is still finely ground for 22-26 hours with absolute ethanol as the medium. After the dried powder passes through a 110-130 mesh sieve, it is formed into a green body under a pressure of 50-200 MPa; d、成型后的坯体在空气中常压下采用埋粉末法烧结，并置于倒放的双坩埚中，烧结温度为1000-1250℃，烧结时间为1-4小时、升温速率为1.5-2.5℃/min；d. The formed green body is sintered in the air under normal pressure by buried powder method, and placed in an inverted double crucible. The sintering temperature is 1000-1250°C, the sintering time is 1-4 hours, and the heating rate is 1.5- 2.5℃/min; e、烧成品经过抛光处理后被银电极，后在硅油中加电压进行极化，极化电压为1.5-3.5kV/mm，极化温度为25-150℃，极化时间为5-30分钟；e. After the fired product is polished, it is covered with a silver electrode, and then polarized by applying a voltage in silicone oil. The polarization voltage is 1.5-3.5kV/mm, the polarization temperature is 25-150°C, and the polarization time is 5-30 minute; f、按照IRE的标准制成压电陶瓷样品进行压电和机电耦合性能的测试。f. According to the standard of IRE, the piezoelectric ceramic samples are made to test the piezoelectric and electromechanical coupling performance.
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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 SnO2 varistor with high nonlinearity, low residual voltage and large current capacity for power system transmission and preparation method thereof
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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 A kind of broadband high-Q low temperature coefficient barium-magnesium-calcium-niobium-tantalum composite ceramic and preparation method thereof
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CN108585851B (en) * 2018-07-10 2021-01-05 合肥工业大学 Sodium niobate-based lead-free potassium-free high-power piezoelectric ceramic and preparation method thereof
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