CN101962292B - 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 PDFInfo
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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
Technical field
The present invention relates to leadless piezoelectric ceramics and preparation method thereof, specifically alkali metal niobium tantalum stibate based leadless piezoelectric ceramics and preparation method thereof.
Background technology
Since over half a century, with lead zirconate titanate (Pb (Zr, Ti) O
3, PZT) for the piezoelectric ceramic of main component has been widely used in electronics, space flight, communication, the military numerous areas that waits.Such as, piezoelectric ceramic is made various filters, oscillator, the electronic components such as trapper.Yet the content of lead oxide or lead orthoplumbate accounts for more than 70% in these piezoceramic materials.Bring serious harm all can in the processing procedure of these leaded piezoelectric ceramic after using and discarding human health and living environment.
Bismuth-sodium titanate is the ferroelectric ceramic 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 forms, have good piezoelectricity and mechanical-electric coupling performance (T.Takenaka, K.Maruyama, and K.Sakata, Jpn.J.Appl.Phys., 30 (1991) 2236; CA1456531A, CN1511800A, CN1673178, JP1999-329533, JP2000-272962).Yet Polarization field strength is higher, and the depolarization 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 to sintering under 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 alkali metal niobium tantalum stibate 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 ceramic form.Barium base cubic perovskite forms 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 alkali metal niobium tantalum stibate 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 alkali metal niobium tantalum stibate 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 characteristic and piezoelectric property.
The technical scheme that technical solution problem of the present invention adopts is:
Alkali metal niobium tantalum stibate based leadless piezoelectric ceramics, its spy is characterised in that: it forms 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 metal ion of tetravalence one or more;
M is selected from the oxide 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 alkali metal niobium tantalum stibate 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 the metal oxide or the carbonate that be used for to mix is raw material, prepares burden according to formula (1);
B, the raw material for preparing be take absolute ethyl alcohol as medium, 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 calcine technology once, finish precalcining synthetic;
The powder of c, pre-synthesis is through after grinding still take absolute ethyl alcohol as medium fine grinding 22-26 hour again, and dried powder crosses that the forming under the pressure at 50-200MPa is 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, heating rate are 1.5-2.5 ℃/min;
E, burn till product through after the polishing by silver electrode, making alive polarizes in silicone oil afterwards, polarizing voltage is 1.5-3.5kV/mm, the polarization temperature is 25-150 ℃, the polarization time is 5-30 minute;
F, make the piezoelectric ceramic sample according to the standard of IRE and carry out piezoelectricity and mechanical-electric coupling performance test.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, pottery of the present invention forms the piezoelectric ceramic of the environment compatibility that is a kind of well behaved unleaded system, can realize substituting the leaded 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 interphase structure of cubic ferroelectric phase by the relative amount of adjusting barium base cubic perovskite and lithium tantalum antimony, thereby reaches excellent piezoelectricity and mechanical-electric coupling performance.
3, leadless piezoelectric ceramics of the present invention repeats batch mixing by twice and calcine technology improves the composition homogeneity with complex component system; and adopt buried powder method and two crucible Protection Code to reduce the volatilization loss of 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 of matrix composition by the doping of the metal oxide of trace, as reduce sintering temperature, improve sintered density, inhibiting grain growth, thereby optimize various piezoelectricity and mechanical-electric 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 electric 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 different temperatures of sample when u=0.005 and v=0.02.
Embodiment
In the implementation, the component that the alkali metal niobium tantalum stibate based leadless piezoelectric ceramics of barium base cubic perovskite modification is expressed by following general formula forms:
(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 metal ion of tetravalence one or more;
M is selected from the oxide 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 alkali metal niobium tantalum stibate based leadless piezoelectric ceramics of above-mentioned barium base cubic perovskite modification is:
With technical pure or chemical pure natrium carbonicum calcinatum (Na
2CO
3), Anhydrous potassium carbonate (K
2CO
3), lithium carbonate (Li
2CO
3), niobium pentaoxide (Nb
2O
5), tantalum pentoxide (Ta
2O
5), antimony pentoxide (Sb
2O
5), barium titanate (BaCO
3), zirconium dioxide (ZrO
2), hafnium oxide (HfO
2), tin ash (SnO
2) and the metal oxide and the carbonate that be used for to mix be raw material, prepare burden according to the composition of general formula (1), finish pre-synthesis through ball mill mixing and calcining successively; The pre-synthesis powder is base substrate through fine grinding and high-pressure molding; Sintering under the normal pressure; Burning till product polarization processes.
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 the metal oxide and the carbonate that be used for to mix is raw material, prepares burden according to formula (1);
2, the raw material for preparing is take absolute ethyl alcohol as medium, 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 calcine technology once, finish precalcining synthetic;
3, the powder of pre-synthesis is through the still again fine grinding 24 hours take absolute ethyl alcohol as medium after grinding, and dried powder crosses that the forming under the pressure at 50-200MPa is 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, heating rate are 2 ℃/min;
5, burn till product through after the polishing by silver electrode, making alive polarizes in silicone oil afterwards, polarizing voltage is 1.5-3.5kV/mm, the polarization temperature is 25-150 ℃, the polarization time is 5-30 minute;
6, make the piezoelectric ceramic sample according to the standard of IRE and carry out piezoelectricity and mechanical-electric coupling performance test.
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 successively each step by above-mentioned execution mode, wherein,
Adopt (1-u) [(Na
0.52K
0.4) (Nb
0.84Sb
0.08) O
3+ (0.08-v) LiTaO
3+ vBaZrO
3The piezoelectric ceramic of]+uCuO for forming, precalcining temperature are that 900 ℃, time are 4 hours.After twice calcining take absolute ethyl alcohol as ball-milling medium ball milling 24 hours again.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=0.01,0.025 and 0.04 o'clock two forms the electric hysteresis loop of sample behind 1150 ℃ of sintering as shown in Figure 4.
Work as u=0.005, v=0.025 and sintering temperature are 1150 ℃, and sintering time is 2 hours, record other physical property such as table 1 of sample:
Table 1
Embodiment 2
Carry out successively each step by above-mentioned execution mode, 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 ceramic that forms during v=0.015, the condition of precalcining is 950 ℃, the time is 3 hours.After twice calcining take absolute ethyl alcohol as ball-milling medium ball milling 24 hours again.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
Embodiment 3
Carry out successively each step by above-mentioned execution mode, 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 ceramic that forms during v=0.02, the condition of precalcining is 1000 ℃, is incubated 3 hours.After twice calcining take absolute ethyl alcohol as ball-milling medium ball milling 24 hours again.And the base substrate of aftershaping is 1200 ℃ of sintering 2 hours, the X-ray diffractogram of its sample under different temperatures as shown in Figure 6, other relevant performance data is listed in table 3:
Table 3
Claims (1)
1. alkali metal niobium tantalum stibate based leadless piezoelectric ceramics is characterized in that: it forms 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;
Me is selected from Zr
4+, Hf
4+, Sn
4+In the metal ion of tetravalence one or more;
M is selected from the oxide of Na, K, Li, Ag, Cu, Fe, Mn, Zn, Nd, Sm, Yb, Sc metal or the carbonate one or more;
Preparation 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 the metal oxide or the carbonate that be used for to mix is raw material, prepares burden according to formula (1);
B, the raw material for preparing be take absolute ethyl alcohol as medium, 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 calcine technology once, finish precalcining synthetic;
The powder of c, pre-synthesis is through after grinding still take absolute ethyl alcohol as medium fine grinding 22-26 hour again, and dried powder crosses that the forming under the pressure at 50-200MPa is 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, heating rate are 1.5-2.5 ℃/min;
E, burn till product through after the polishing by silver electrode, making alive polarizes in silicone oil afterwards, polarizing voltage is 1.5-3.5kV/mm, the polarization temperature is 25-150 ℃, the polarization time is 5-30 minute;
F, make the piezoelectric ceramic sample according to the standard of IRE and carry out piezoelectricity and mechanical-electric coupling performance test.
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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 |
| JP7271376B2 (en) * | 2019-09-13 | 2023-05-11 | 株式会社東芝 | Composite oxides, active material composites, electrodes, batteries, battery packs, and vehicles |
| CN110668808B (en) * | 2019-10-17 | 2022-07-22 | 新疆大学 | SnO with high nonlinearity, low residual voltage and large through-current capacity for power transmission of power system2Preparation method of piezoresistor |
| 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 |
| CN112341160B (en) * | 2020-11-06 | 2022-08-30 | 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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| 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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| CN101024574A (en) * | 2007-01-30 | 2007-08-29 | 合肥工业大学 | Sodium-potassium niobate series substituted by bismuth-base calcium-titanium ore and preparing method |
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