CN101024573A - Multi-element sodium-potassium niobate series lead-free piezoelectric ceramic and preparing method - Google Patents
Multi-element sodium-potassium niobate series lead-free piezoelectric ceramic and preparing method Download PDFInfo
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- CN101024573A CN101024573A CN 200710019869 CN200710019869A CN101024573A CN 101024573 A CN101024573 A CN 101024573A CN 200710019869 CN200710019869 CN 200710019869 CN 200710019869 A CN200710019869 A CN 200710019869A CN 101024573 A CN101024573 A CN 101024573A
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Abstract
The invention relates to a multielement potassium niobate natrium series leadless piezoelectric ceramics and the manufacturing method. It is expressed by the general equation: (1-u)[(1-z-n)(LitNa1-w-t1Kw-t2)(Nb1-g-fTagSbf)O3+ z(Bi0.5Na0.5xK0.5 (1-x))TiO3+nBaTiO3]+uM. The invention has stable manufacturing technology and has great usefulness.
Description
Technical field
The present invention relates to lead-free piezoelectric ceramic composition and preparation method thereof, more particularly relate to a kind of with bismuth-sodium titanate ((Bi
0.5Na
0.5) TiO
3), bismuth potassium titanate (((Bi
0.5K
0.5) TiO
3)), barium titanate (BaTiO
3) and potassium-sodium niobate ((Na.K) NbO
3) the sosoloid leadless piezoelectric ceramics that forms and preparation method thereof.
Background technology
Piezoelectric ceramics has spreaded all over the every nook and cranny in people's daily life as a most widely used class material in the function ceramics field, and a large amount of application is militarily also arranged.As the various wave filters that piezoelectric ceramics is made, vibrator, electronic components such as wavetrap.Yet these piezoceramic materials mainly are that (Pb (Zr, Ti) O3) is a main component with Pb-based lanthanumdoped zirconate titanates for many years.Wherein the content of plumbous oxide or tri-lead tetroxide accounts for raw-material more than 70%.Bring serious harm all can in the treating processes of these plumbiferous piezoelectric ceramics after using and discarding human beings'health and living environment.The piezoelectricity ferro pottery that develops the environment compatibility of unleaded system be one urgent and have a problem of great Practical significance.
Bismuth-sodium titanate ((Bi
0.5Na
0.5) TiO
3, be called for short BST) and be the compound leadless piezoelectric material material in a kind of A position with perovskite structure, be the ferroelectric ceramic(s) of a kind of research unleaded type early.Its single crystal has very big residual polarization (P
r=38 μ C/cm
2) and very high coercive field (E
c=7.3kV/mm), however polarization is quite difficult, and the umpolarization temperature is lower, has limited its practical application.Bismuth potassium titanate (((Bi
0.5Na
0.5) TiO
3)) be a kind ofly rare to have cubic perovskite structure and Curie temperature reaches 380 ℃ non-plumbum ferroelectric material, it and BST and BST and BT form accurate homotype phase boundary and form, have good piezoelectricity and electromechanical coupling performance (A.Sadaki, T.Chiba, Y.Mamiya, and E.Otsuki, Jpn.J.Appl.Phys.38 (1999) 5564; T.Takenaka, K.Maruyama, and K.Sakata, Jpn.J.Appl.Phys., 30 (1991) 2236).
Recently, 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) and obtain extensive studies, have bigger piezoelectricity and electromechanical coupling performance, bigger Curie temperature (T
c=420 ℃).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.
Above-mentioned two kinds of lead-free systems are that at present research is more, and the leadless piezoelectric candidate material with very big potentiality, yet because inherent shortcoming separately, the application that distance is actual also still has distance.Yet there are no the electrical property of the piezoelectric ceramic composition of forming by these two kinds of typical leadless piezoelectric material materials and preparation technology's research report in the existing document.
Summary of the invention
The present invention is for avoiding above-mentioned existing in prior technology weak point, a kind of multi-element sodium-potassium niobate series lead-free piezoelectric ceramic and preparation method thereof is provided, this pottery composition has good piezo-electric modulus, can practical planar electromechanical coupling factor and high Curie temperature.
The technical scheme that the present invention is adopted for the technical solution problem is:
Multi-element sodium-potassium niobate series lead-free piezoelectric ceramic of the present invention is characterized in that it is made up of following general formula to express:
(1-u)[(1-z-n)(Li
tNa
1-w-t1K
w-t2)(Nb
1-g-fTa
gSb
f)O
3+z(Bi
0.5Na
0.5xK
0.5(1-x))TiO
3+nBaTiO
3]+uM..(1)
X, z, u, n, w, g, f, t, t1 and t2 are each element shared atomic percent in material component in the general formula (1), and: 0≤x≤1,0＜z≤0.08,0.3≤w≤0.7,0≤u≤0.02,0≤n≤0.09,0≤g≤0.12,0≤f≤0.12,0≤t≤0.06, and t1+t2=t, satisfy t1 〉=0 simultaneously, t2 〉=0;
M is at least a oxide compound or the carbonate that is selected from following metal, Na, K, Li, Ag, Ta, Sb, Al, Cu, Fe, Mn, Zn, Pr, Nd, Sm, Gd, La, Dy, Er, Yb, Sc, Ca, Ba, Sr, Mg.
The preparation method of multi-element sodium-potassium niobate series lead-free piezoelectric ceramic of the present invention is characterized in that:
With 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), bismuthous oxide bismuth trioxide (Bi
2O
3) and titanium dioxide (TiO
2) and be used for adulterated metal oxide or carbonate is raw material, according to the composition batching of general formula (1), 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 burns till product polarization processing.
Preparation method's of the present invention characteristics also are to carry out as follows:
A, with anhydrous sodium carbonate, Anhydrous potassium carbonate, Quilonum Retard, Niobium Pentxoxide, tantalum pentoxide, antimony peroxide, bismuthous oxide bismuth trioxide and titanium dioxide, and be used for adulterated metal oxide or carbonate is raw material are according to the composition batching of general formula (1);
B, confected materials are medium with the dehydrated alcohol, through behind 8-16 hour the ball mill mixing, drying obtains dry powder; Gained dry powder temperature with 800-950 ℃ in alumina crucible was calcined 2-6 hour; Repeat the calcining of ball mill mixing and dry powder once, it is synthetic to finish precalcining;
C, pre-synthetic powder be 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;
D, base substrate adopt under the normal pressure in air and bury the powder method sintering, and sintering temperature is 1000-1150 ℃, and sintering time is that 1-4 hour, temperature rise rate are 2 ℃/min;
By silver electrode, the back is the making alive polarization in silicone oil after the sample process polished finish behind e, the sintering, and polarizing voltage is 2-3kV/mm, and the polarization temperature is 25-150 ℃, and the polarization time is 10-30 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, the present invention's pottery is formed the piezoelectricity ferro pottery of the environment compatibility that is a kind of well behaved unleaded system, and its stable preparation process also can adopt the technology of preparing of conventional piezoelectric pottery and industrial raw material to obtain, and has practicality.
2, the present invention by adjusting lithium content and titanate in the ratio of barium, potassium and sodium, the pottery that can obtain to have accurate homotype phase boundary structure is formed, thereby reaches excellent piezoelectricity and electromechanical coupling performance;
3, pottery composition of the present invention can obtain a kind of density height, the leadless piezoelectric ceramics of titanate that piezoelectric property is good and potassium-sodium niobate system solid solution by controlling preparation technology and sintering schedule such as temperature and time;
4, ceramic formula of the present invention effectively improves sintering behavior that matrix forms as reducing sintering temperature in the doping of the metal oxide by trace, improve sintered density, suppress grain growth, improve the deliquescence characteristic of pottery and improve various piezoelectricity and the electromechanical coupling performance.
Description of drawings
Fig. 1 consists of 0.97 (Na in the embodiment of the invention 1
0.5K
0.5) Nb0
3+ 0.03 (Bi
0.5K
0.5) TiO
3, at 2 hours sample stereoscan photograph of 1080 ℃ sintering temperatures.
Fig. 2 consists of 0.98 (Na in the embodiment of the invention 2
0.5K
0.5) NbO
3+ 0.02 (Bi
0.5Na
0.5) TiO
3, at 2 hours sample electromicroscopic photograph of 1090 ℃ of sintering.
Fig. 3 consists of 0.98 (Na in the embodiment of the invention 3
0.475K
0.475Li
0.05) NbO
3+ 0.02 (Bi
0.48Na
0.48Ba
0.04) TiO
3, at 2 hours sample electromicroscopic photograph of 1080 ℃ of sintering.
Fig. 4 consists of 0.97 (Na in the embodiment of the invention 1
0.5K
0.5) NbO
3+ 0.03 (Bi
0.5K
0.5) TiO
3, the dielectric-temperature curve when 1M Hz.
Fig. 5 consists of 0.98 (Na in the embodiment of the invention 2
0.5K
0.5) NbO
3+ 0.02 (Bi
0.5Na
0.5) TiO
3, the dielectric-temperature curve when 100kHz.
Fig. 6 consists of 0.98 (Na in the embodiment of the invention 3
0.475K
0.475Li
0.05) NbO
3+ 0.02 (Bi
0.48Na
0.48Ba
0.04) TiO
3, the dielectric-temperature curve when 1M Hz.
Embodiment
By (1-u) [(1-z-n) (Li
tNa
1-w-t1K
W-t2) (Nb
1-g-fTa
gSb
f) O
3+ z (Bi
0.5Na
0.5xK
0.5 (1-x)) TiO
3+ nBaTiO
3]+uM calculates the consumption of each component, and takes by weighing raw material with analytical balance.
X in the formula, z, u, n, w, g, f, t, t1 and t2 are each element shared atomic percent in material component,
And: 0≤x≤1,0＜z≤0.08,0.3≤w≤0.7,0≤u≤0.02,0≤n≤0.09,0≤g≤0.12,0≤f≤0.12,0≤t≤0.06, and t1+t2=t, satisfy t1 〉=0 simultaneously, t2 〉=0;
M is at least a oxide compound or the carbonate that is selected from following metal, Na, K, Li, Ag, Ta, Sb, Al, Cu, Fe, Mn, Zn, Pr, Nd, Sm, Gd, La, Dy, Er, Yb, Sc, Ca, Ba, Sr, Mg.
Preparation process is as follows:
1, with 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, bismuthous oxide bismuth trioxide Bi
2O
3With titanium dioxide TiO
2, and be used for adulterated metal oxide or carbonate is raw material, according to the composition batching of general formula (1);
2, confected materials is medium with the dehydrated alcohol, through behind 8-16 hour the ball mill mixing, drying obtains dry powder; Gained dry powder temperature with 800-950 ℃ in alumina crucible was calcined 2-6 hour; Repeat the calcining of ball mill mixing and dry powder once, to promote the uniform distribution of component, 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, base substrate adopts under the normal pressure in air and buries the powder method sintering, and sintering temperature is 1000-1150 ℃, and sintering time is that 1-4 hour, temperature rise rate are 2 ℃/min;
5, the sample behind the sintering through after the polished finish by silver electrode, the back is the making alive polarization in silicone oil, polarizing voltage is 2-3kV/mm, the polarization temperature is 25-150 ℃, the polarization time is 10-30 minute;
6, make the test that the piezoelectric ceramics sample carries out piezoelectricity and electromechanical coupling performance according to the standard of IRE.
Embodiment 1: carry out each step successively by above-mentioned embodiment, wherein
In the step 1, press x=0, z=0.03, w=0.5, f=0, g=0, u=0, n=0, t1=0 and t2=0 carry out value,
The composition general formula is expressed as: 0.97 (Na
0.5K
0.5) NbO
3+ 0.03 (Bi
0.5K
0.5) TiO
3
In the step 2, calcining temperature is 900 ℃, and calcination time is 5 hours;
In the step 4, the blank sintering temperature is 1080 ℃, and sintering time is 2 hours.
The stereoscan photograph of the sample natural surface that obtains as shown in Figure 1, the dielectric-temperature characteristics of sample such as Fig. 4, the physical performance data that other is relevant:
Density (g/cm
2) grain-size (μ m) ε
33/ ε
o(1kHz) d
33(pC/N) k
p(%)
4.31 3.2 850 191 45
Embodiment 2: carry out each step successively by above-mentioned embodiment, wherein
In the step 1, press x=1, z=0.02, w=0.5, u=0, n=0, g=0, f=0, t1=0 and t2=0 carry out value,
The composition general formula is expressed as: 0.98 (Na
0.5K
0.5) NbO
3+ 0.02 (Bi
0.5Na
0.5) TiO
3
In the step 2, calcining temperature is 850 ℃, and calcination time is 5 hours;
In the step 4, the blank sintering temperature is 1090 ℃, and sintering time is 2 hours.
The stereoscan photograph of the sample natural surface that obtains as shown in Figure 2, the dielectric-temperature characteristics of sample such as Fig. 5, the physical performance data that other is relevant:
Density (g/cm
2) grain-size (μ m) ε
33/ ε
o(1kHz) d
33(pC/N) k
p(%)
4.33 2.2 600 185 43
Embodiment 3: carry out each step successively by above-mentioned embodiment, wherein
In the step 1, press x=1, z=0.0192, w=0.5, u=0, n=0.0008, g=0, f=0, t1=0.025 and t2=0.025 carry out value,
The composition general formula is expressed as: 0.98 (Na
0.475K
0.475Li
0.05) NbO
3+ 0.02 (Bi
0.48Na
0.48Ba
0.04) TiO
3
In the step 2, calcining temperature is 950 ℃, and calcination time is 5 hours;
In the step 4, the blank sintering temperature is at 1080 ℃, and sintering time is 2 hours.
The stereoscan photograph of the sample natural surface that is obtained as shown in Figure 3, the dielectric-temperature characteristics of sample such as Fig. 6, the physical performance data that other is relevant:
Density (g/cm
2) grain-size (μ m) ε
33/ ε
o(1kHz) d
33(pC/N) k
p(%)
4.36 2.5 700 235 47
Embodiment 4: carry out each step successively by above-mentioned embodiment, wherein
In the step 1, press x=1, z=0.02, w=0.5, u=0.005, n=0, g=0, f=0, t1=0 and t2=0 carry out value,
M is: Fe
2O
3
The composition general formula is expressed as: 0.9751 (Na
0.5K
0.5) NbO
3+ 0.0199 (Bi
0.5Na
0.5) TiO
3+ 0.005Fe
2O
3
In the step 2, calcining temperature is 850 ℃, and calcination time is 5 hours;
In the step 4, the blank sintering temperature is 1090 ℃, and sintering time is 2 hours, and relevant physical performance data is:
Density (g/cm
2) grain-size (μ m) ε
33/ ε
o(1kHz) d
33(pC/N) k
p(%)
4.35 3.0 620 190 42
Embodiment 5: carry out each step successively by above-mentioned embodiment, wherein
In the step 1, press x=1, z=0.0192, w=0.5, u=0, n=0.0008, g=0.08, f=0.02, t1=0.025 and t2=0.025 carry out value,
The composition general formula is expressed as:
0.98(Na
0.475K
0.475Li
0.05)(Nb
0.90Ta
0.08Sb
0.02)O
3+0.02(Bi
0.48Na
0.48Ba
0.04)TiO
3
In the step 2, calcining temperature is 830 ℃, and calcination time is 6 hours;
In the step 4, the blank sintering temperature is 1080 ℃, and sintering time is 3 hours, and relevant physical performance data is:
Density (g/cm
2) grain-size (μ m) ε
33/ ε
o(1kHz) d
33(pC/N) k
p(%)
4.35 2.3 850 320 46
Claims (3)
1, multi-element sodium-potassium niobate series lead-free piezoelectric ceramic is characterized in that it is made up of following general formula to express:
(1-u)[(1-z-n)(Li
tNa
1-w-t1K
w-t2)(Nb
1-g-fTa
gSb
f)O
3+z(Bi
0.5Na
0.5xK
0.5(1-x))TiO
3+nBaTiO
3]+uM..(1)
X, z, u, n, w, g, f, t, t1 and t2 are each element shared atomic percent in material component in the general formula (1), and: 0≤x≤1,0＜z≤0.08,0.3≤w≤0.7,0≤u≤0.02,0≤n≤0.09,0≤g≤0.12,0≤f≤0.12,0≤t≤0.06, and t1+t2=t, satisfy t1 〉=0 simultaneously, t2 〉=0;
M is at least a oxide compound or the carbonate that is selected from following metal, Na, K, Li, Ag, Ta, Sb, Al, Cu, Fe, Mn, Zn, Pr, Nd, Sm, Gd, La, Dy, Er, Yb, Sc, Ca, Ba, Sr, Mg.
2, the preparation method of the described multi-element sodium-potassium niobate series lead-free piezoelectric ceramic of a kind of claim 1 is characterized in that:
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), bismuthous oxide bismuth trioxide (Bi
2O
3), titanium dioxide (TiO
2) and be used for adulterated metal oxide or carbonate is raw material, according to the composition batching of general formula (1), 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 burns till product polarization processing.
3, method according to claim 2 is characterized in that carrying out as follows:
A, with anhydrous sodium carbonate, Anhydrous potassium carbonate, Quilonum Retard, Niobium Pentxoxide, tantalum pentoxide, antimony peroxide, bismuthous oxide bismuth trioxide and titanium dioxide and be used for adulterated metal oxide or carbonate is raw material are according to the composition batching of general formula (1);
B, confected materials are medium with the dehydrated alcohol, through behind 8-16 hour the ball mill mixing, drying obtains dry powder; Gained dry powder temperature with 800-950 ℃ in alumina crucible was calcined 2-6 hour; Repeat the calcining of ball mill mixing and dry powder once, it is synthetic to finish precalcining;
C, pre-synthetic powder be 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;
D, base substrate adopt under the normal pressure in air and bury the powder method sintering, and sintering temperature is 1000-1150 ℃, and sintering time is that 1-4 hour, temperature rise rate are 2 ℃/min;
By silver electrode, the back is the making alive polarization in silicone oil after the sample process polished finish behind e, the sintering, and polarizing voltage is 2-3kV/mm, and the polarization temperature is 25-150 ℃, and the polarization time is 10-30 minute;
F, make the test that the piezoelectric ceramics sample carries out piezoelectricity and electromechanical coupling performance according to the standard of IRE.
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|---|---|---|---|
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