CN101269962B - Niobate base leadless piezoelectric ceramic with high tension electricity coefficient and preparation method thereof - Google Patents
Niobate base leadless piezoelectric ceramic with high tension electricity coefficient and preparation method thereof Download PDFInfo
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Abstract
The present invention provides niobate-based lead-free piezoelectric ceramics of high piezoelectric coefficient, which is shown in the general formula (1-z)(Nav-tKu-x-wLixHwAgt)(Nb1-x-y-wTaxSbyTiw)O3.zM Alpha O Beta; wherein, v is more than 0,5 and less than 0.6; w is more than or equal to 0 and less than 0.02; v plus u is 1; t is more than or equal to 0 and less than 0.03; x is more than 0.02 and less than 0.07; y is more than 0.03 and less than 0.08; z is more than or equal to 0 and less than 5; x, y, u, v, w and t stand for atomic percent of each element in the ingredients; z stands for the weight percent of oxides in the ingredients; H is selected from at least one of Ba, Mg, Sr and Ca; M Alpha O Beta is one oxide or a plurality of mixed oxides; the value of M is 1 to 6, and M is an element that can form a solid oxide with oxygen. The preparation method comprises mixing raw materials, presintering, granulation, preparing bisque, dumping, sintering, silver coating, and polarization. In the lead-free piezoelectric ceramics, the d33 can reach 350pC/N; the kp can reach 50 percent; the dielectric constant Epsilon r is 1550; the tangent tan Delta of the loss angle is less than 0.03;the Tc can reach 310 DEG C; the time stability is excellent; and the process is simple. And the lead-free piezoelectric ceramics can be used for preparing drives, sound generators, ultrasonic transducer, resonator and other devices.
Description
One, technical field
The present invention relates to a kind of ceramic material and preparation method thereof, specifically a kind of niobate base lead-free piezoelectric ceramic and preparation method thereof with high tension electricity coefficient.
Two, background technology
The piezoceramic material that generally is used for many years mainly is with Pb-based lanthanumdoped zirconate titanates (Pb (Zr, Ti) O
3) be main component, wherein the content of plumbous oxide or tri-lead tetroxide accounts for raw-material more than 60%.Bring serious harm all can in the treating processes of these plumbiferous piezoelectric ceramics after using and discarding human beings'health and living environment.
Leadless piezoelectric ceramics mainly contains barium phthalate base (BaTiO usually
3, be called for short BT), bismuth sodium titanate based ((Bi
0.5Na
0.5) TiO
3, be called for short BNT), potassium-sodium niobate-based ((K, Na) NbO
3, be called for short KNN), tungsten bronze structure and bismuth laminated ferroelectric material.Wherein BT is the piezoelectric ceramics that early obtains using, but because its piezoelectric property is low, particularly Curie temperature is on the low side, greatly limits its use.BNT is the compound leadless piezoelectric material material with perovskite structure in a kind of A position, it is the ferroelectric ceramic(s) of a kind of research unleaded type early, it and BT form accurate homotype phase boundary and form, have good piezoelectricity and electromechanical coupling performance (T.Takenaka, K.Maruyama, and K.Sakata, Jpn.J.Appl.Phys., 30 (1991) 2236), yet, very high coercive field (E
c=7.3 kV/mm), make quite difficulty of its polarization, and the umpolarization temperature is lower, has limited its practical application.
Be that the pottery of main component has obtained paying attention to widely and studying recent years with the base metal niobate.The pottery of this individual system has bigger piezoelectricity and electromechanical coupling performance usually, and high Curie temperature demonstrates huge application potential.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.Although by various doping vario-properties, its piezoelectric property is effectively improved, yet the process repeatability of this class pottery is poor at present, potassium sodium is volatile to be caused stoichiometric departing from, and physical strength is low, and the temperature stability of piezoelectricity and electromechanical properties is not enough.At present,, carried out number of research projects, comprised and seek new potassium-sodium niobate-based composition with accurate homotype phase boundary at this material system; The A position stoichiometry in the basic metal niobium tantalum stibnate system and the adjustment of K/Na ratio; Regulate the relative content of lithium, tantalum and antimony; Improve the thermostability of its electrical property; Optimize sintering process, powder preparing technology and electropolarization technology; Texturing technology etc.Although these research work in electrical property that to a certain degree improves this individual system lead-free piezoceramic material and stability, are still waiting further raising yet compare its piezoelectric property with PZT base composition, as d
33On the low side, electromechanical coupling factor deficiency etc.All these greatly limits the practical application of this leadless piezoelectric material material in device.
Three, summary of the invention
The present invention aims to provide a kind of niobate base lead-free piezoelectric ceramic with high tension electricity coefficient for avoiding above-mentioned existing in prior technology weak point, and technical problem to be solved is that pottery is formed and structure Design, and optimization of preparation.
The technical scheme that the present invention is adopted for the technical solution problem is:
A kind of niobate base lead-free piezoelectric ceramic with high tension electricity coefficient that the present invention is alleged, characteristics are that it is made up of following general formula expression:
(1-z)(Na
v-tK
u-x-wLi
xH
wAg
t)(Nb
1-x-y-wTa
xSb
yTi
w)O
3·zM
αO
β…………………………(1)
X, y, u, v, w, t are each element shared atomic percent in material component in the general formula (1), and z is the mass percent that oxide weight accounts for the raw material total amount; 0.5＜v＜0.6,0≤w＜0.02, v+u=1,0≤t＜0.03,0.02＜x＜0.07,0.03＜y＜0.08,0≤z＜5%.
Wherein, H is for being selected from a kind of of following metallic element: Ba (barium), Mg (magnesium), Sr (strontium), Ca (calcium) at least; The M that is added
αO
βBe one or more doping oxides, M is+1～+ 6 valency and the element that can form solid-oxide with oxygen, is selected from down at least a element: Na (sodium) in the column element, K (potassium), Li (lithium), Ag (silver), Al (aluminium), Cu (copper), Fe (iron), Mn (manganese), Zn (zinc), Pr (praseodymium), Nd (neodymium), Si (silicon), Sm (samarium), Gd (gadolinium), La (lanthanum), Bi (bismuth), Dy (dysprosium), Er (erbium), Yb (ytterbium), Sc (scandium), Sb (antimony), Nb (niobium), V (vanadium), Ta (tantalum) and W (tungsten).α and β represent the atomicity of corresponding element M and O in the relevant oxide compound respectively.
Preparation method with niobate base lead-free piezoelectric ceramic of high tension electricity coefficient of the present invention, comprise raw material mixing, pre-burning, granulation, making biscuit, binder removal, sintering, quilt silver, polarization step, difference with the prior art is with a certain amount of 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), antimonous oxide (Sb
2O
3), be medium ball milling 4～18 hours with the dehydrated alcohol, obtain compound; To calcine 2～6 hours down in 800～950 ℃ after the compound drying, the synthetic synthetic material that obtains is once finished in ball milling, drying, calcining at least again; In synthetic material, add an amount of binding agent in order to granulation; Sample after the moulding obtained the porcelain base through behind the binder removal in 1～4 hour in 1000～1100 ℃ of following sintering; The porcelain base is polished by the processing 10～30 minutes that polarizes in silicone oil after the silver electrode, polarizing voltage 2～4kv/mm, 20～150 ℃ of polarization temperature.
Described " a certain amount of " (each raw material) is exactly the amount that takes by weighing after measuring in the ratio of composition shown in the general formula (1) and qualification thereof.
When mixing, raw material can also add a certain amount of titanium dioxide (TiO
2) and alkaline earth metal carbonate such as barium carbonate (BaCO
3) or/and Strontium carbonate powder (SrCO
3) or/and lime carbonate (CaCO
3) or/and magnesiumcarbonate (MgCO
3) one mixing and ball milling, so-called " a certain amount of " implication is the same.
When mixing, raw material can also add a certain amount of silver carbonate (Ag
2CO
3) one mixing and ball milling.So-called " a certain amount of " implication is the same.
Oxide compound or one mixing and ball milling of carbonate that when raw material mixes, can also add a certain amount of doped element M.So-called " a certain amount of " (material mixes) implication is the same.
Concrete preparation technology is as follows:
A, with anhydrous sodium carbonate, Anhydrous potassium carbonate, Quilonum Retard, barium carbonate (or Strontium carbonate powder, lime carbonate, magnesiumcarbonate), titanium dioxide, silver carbonate, Niobium Pentxoxide, tantalum pentoxide, antimonous oxide and be used for the oxide compound of doped element M or raw material such as carbonate, according to the composition of general formula (1) and the ratio metering weighing batching of qualification;
B, confected materials are medium with the dehydrated alcohol, and after ball milling obtained the ball milling compound in 4～18 hours, dry back temperature with 800～950 ℃ in alumina crucible was calcined 2～6 hours; Repeat the calcining of ball mill mixing and dry powder once, finish the pre-synthetic synthetic material that obtains of calcining;
C, synthetic material pass through once more ball-milling technology levigate after, add the binding agent granulation, again through moulding and binder removal, be to obtain the porcelain base in 1～4 hour 1000～1100 ℃ of sintering temperature times at last;
D, with the porcelain base through after the polished finish by silver electrode, the back is the making alive polarization in silicone oil, polarizing voltage is 2～4kV/mm, the polarization temperature is 25～150 ℃, the polarization time is 10～30 minutes;
E, make the test that the piezoelectric ceramics sample carries out piezoelectricity and electromechanical coupling performance according to the standard of IRE.
A kind of niobate base lead-free piezoelectric ceramic that the present invention proposes and preparation method thereof with high tension electricity coefficient, its beneficial effect is embodied in:
1, the present invention pottery is formed the piezoelectric ceramics of the environment compatibility that is a kind of unleaded system with high tension electricity coefficient, 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 is by the content of adjusting potassium/sodium ratio, silver, antimony, tantalum, titanates of alkali-earth metals and the doping vario-property of an amount of oxide compound, can obtain to be positioned near the pottery of accurate homotype phase boundary forms, thereby reach excellent piezo-electric modulus and can practical plane electromechanical coupling performance, excellent mechanical intensity and temperature stability.
3, the d of this leadless piezoelectric ceramics
33Can reach 350pC/N, k
pCan reach 50%, DIELECTRIC CONSTANT
rBe 1550, losstangenttan＜0.03, T
cCan be up to 310 ℃; And time stability is good, and technology is simple, can be used for making the material of devices such as driving mechanism, rattler, ultrasonic transducer, resonator.
Four, description of drawings
Fig. 1 consists of (Na in the embodiment of the invention 1
0.518K
0.432Li
0.045Ag
0.005) (Nb
0.90Ta
0.045Sb
0.55) O
3, at the stereoscan photograph of 1090 ℃ sintering temperatures sample after 3 hours.
Fig. 2 consists of (Na in the embodiment of the invention 2
0.510K
0.44Li
0.04Ag
0.005Ba
0.005) (Nb
0.895Ta
0.04Sb
0.06Ti
0.005) O
3Specific inductivity-the temperature curve of the ceramics sample of+0.2wt%CuO under different frequency.
Five, embodiment
According to prescription (1-z) (Na
V-tK
U-x-wLi
xH
wAg
t) (Nb
1-x-y-wTa
xSb
yTi
w) O
3ZM
αO
βCalculate the consumption of each component, raw materials by weight is taken by weighing.
X, y, u, v, w, t are each element shared atomic percent in material component in the formula, and z is the mass percent that oxide weight accounts for the raw material total amount; 0.5＜v＜0.6,0≤w＜0.02, v+u=1,0≤t＜0.03,0.02＜x＜0.07,0.03＜y＜0.08,0≤z＜5%.
Wherein, H is for being selected from a kind of of following metallic element: Ba, Mg, Sr, Ca at least; The M that is added
αO
βBe one or more doping oxides, M is+1～+ 6 valency and the element that can form solid-oxide with oxygen, is selected from down in the column element at least a: Na, K, Li, Ag, Al, Cu, Fe, Mn, Zn, Pr, Nd, Si, Sm, Gd, La, Bi, Dy, Er, Yb, Sc, Sb, Nb, V, Ta and W.α and β represent the atomicity of corresponding element M and O in the relevant oxide compound respectively.In preparation technology, M adds with the form of its oxide compound or carbonate raw material.
Preparation technology's concrete steps are as follows:
1, with anhydrous sodium carbonate, Anhydrous potassium carbonate, Quilonum Retard, barium carbonate (or Strontium carbonate powder, lime carbonate, magnesiumcarbonate), titanium dioxide, silver carbonate, Niobium Pentxoxide, tantalum pentoxide, antimonous oxide and be used for the oxide compound of doped element M or raw material such as carbonate, according to the composition of general formula (1) and the ratio metering weighing batching of qualification;
2, confected materials is medium with the dehydrated alcohol, and after ball milling obtained the ball milling compound in 4～18 hours, dry back temperature with 800～950 ℃ in alumina crucible was calcined 2～6 hours; Repeat the calcining of ball mill mixing and dry powder once, finish the pre-synthetic synthetic material that obtains of calcining;
3, synthetic material pass through once more ball-milling technology levigate after, add the binding agent granulation, again through moulding and binder removal, be to obtain the porcelain base in 1～4 hour 1000～1100 ℃ of sintering temperature times at last;
4, with the porcelain base through after the polished finish by silver electrode, the back is the making alive polarization in silicone oil, polarizing voltage is 2～4kV/mm, the polarization temperature is 25～150 ℃, the polarization time is 10～30 minutes;
5, 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 v=0.523, t=0.005, x=0.045, y=0.055, z=0 carries out value.The expression formula of composition is: (Na
0.518K
0.432Li
0.045Ag
0.005) (Nb
0.90Ta
0.045Sb
0.055) O
3
In the step 2, calcining temperature is 900 ℃, and calcination time is 5h;
In the step 3, sintering temperature is 1080 ℃, and sintering time is 3h;
The stereoscan photograph of the sample natural surface that obtains as shown in Figure 1, performance such as table 1 that other is relevant:
Table 1
| Density (g/cm 2) | T c(℃) | d 33(pC/N) | k p(％) |
| 4.32 | 315 | 351 | 50 |
Embodiment 2: carry out each step successively by above-mentioned embodiment, wherein
In the step 1, press v=0.515, t=0.005, w=0.005, x=0.04, y=0.06, z=0.2% carries out value.The expression formula of composition is: (Na
0.510K
0.44Li
0.04Ag
0.005Ba
0.005) (Nb
0.895Ta
0.04Sb
0.06Ti
0.005) O
30.2wt%CuO;
In the step 2, calcining temperature is 860 ℃, and calcination time is 5h;
In the step 3, sintering temperature is 1070 ℃, and sintering time is 3h;
The preparation the leadless piezoelectric ceramics sample the specific inductivity under different frequency to the variation of temperature curve as shown in Figure 2, other correlated performance such as table 2:
Table 2
| Density (g/cm 2) | T c(℃) | d 33(pC/N) | k p(％) |
| 4.39 | 310 | 348 | 49 |
Embodiment 3: carry out each step successively by above-mentioned embodiment, wherein
In the step 1, press v=0.515, t=0.005, w=0.005, x=0.04, y=0.06, z=0.2% carries out value.The expression formula of composition is: (Na
0.510K
0.44Li
0.04Ag
0.005Ba
0.005) (Nb
0.895Ta
0.04Sb
0.06Ti
0.005) O
30.2wt%MnO
2
In the step 2, calcining temperature is 860 ℃, and calcination time is 5h;
In the step 3, sintering temperature is 1070 ℃, and sintering time is 3h;
The correlated performance such as the table 3 of the leadless piezoelectric ceramics sample of preparation:
Table 3
| Density (g/cm 2) | T c(℃) | d 33(pC/N) | k p(％) |
| 4.38 | 308 | 335 | 48 |
Embodiment 4: carry out each step successively by above-mentioned embodiment, wherein
In the step 1, press v=0.523, t=0.005, x=0.045, y=0.055, z=0.25% carries out value.The expression formula of composition is: (Na
0.518K
0.432Li
0.045Ag
0.005) (Nb
0.90Ta
0.045Sb
0.055) O
30.25%Fe
2O
3
In the step 2, calcining temperature is 900 ℃, and calcination time is 5h;
In the step 3, sintering temperature is 1060 ℃, and sintering time is 2h;
The correlated performance such as the table 4 of the leadless piezoelectric ceramics sample of preparation:
Table 4
| Density (g/cm 2) | T c(℃) | d 33(pC/N) | k p(％) |
| 4.41 | 314 | 345 | 48 |
Claims (6)
1. the niobate base lead-free piezoelectric ceramic of a high tension electricity coefficient, its composition is expressed by following general formula (1):
(1-z)(Na
v-tK
u-x-wLi
xH
wAg
t)(Nb
1-x-y-wTa
xSb
yTi
w)O
3·zM
αO
β……………………………(1)
X, y, u, v, w, t are each element shared atomic percent in material component in the general formula (1), and z is the mass percent that oxide weight accounts for the raw material total amount; 0.5＜v＜0.6,0≤w＜0.02, v+u=1,0≤t＜0.03,0.02＜x＜0.07,0.03＜y＜0.08,0≤z＜5%;
Wherein, H is for being selected from a kind of of following metallic element: Ba, Mg, Sr, Ca at least;
M
αO
βBe one or more doping oxides, M is+1～+ 6 valency and the element that can form solid-oxide with oxygen, be selected from down in the column element at least a: Cu, Fe, Mn, Zn, Si, Bi, V and W, α and β represent the atomicity of corresponding element M and O in the relevant oxide compound respectively.
2. by the preparation method of the niobate base lead-free piezoelectric ceramic of the described high tension electricity coefficient of claim 1, comprise raw material mixing, pre-burning, granulation, making biscuit, binder removal, sintering, quilt silver, polarization, it is characterized in that: described mixing and ball milling is anhydrous sodium carbonate, Anhydrous potassium carbonate, Quilonum Retard, Niobium Pentxoxide, tantalum pentoxide, the antimonous oxide with metering, with the dehydrated alcohol is medium ball milling 4～18 hours, obtains compound; To calcine 2～6 hours down in 800～950 ℃ after the compound drying, the synthetic synthetic material that obtains is once finished in ball milling, drying, calcining at least again; In synthetic material, add an amount of binding agent in order to granulation; Sample after the moulding obtained the porcelain base through behind the binder removal in 1～4 hour in 1000～1100 ℃ of following sintering; The porcelain base is polished by the processing 10～30 minutes that polarizes in silicone oil after the silver electrode, polarizing voltage 2～4kv/mm, 20～150 ℃ of polarization temperature.
3. preparation method according to claim 2 is characterized in that: the titanium dioxide that when raw material mixes, adds metering with barium carbonate or/and Strontium carbonate powder or/and lime carbonate or/and the magnesiumcarbonate ball milling.
4. according to claim 2 or 3 described preparation methods, it is characterized in that: one ball milling of silver carbonate that when raw material mixes, adds metering.
5. preparation method according to claim 4 is characterized in that: oxide compound or one ball milling of carbonate of adding the doped element M of metering when raw material mixes.
6. according to claim 2 or 5 described preparation methods, it is characterized in that: before the synthetic material granulation at least again ball milling and the calcining once.
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| CN101798201B (en) * | 2010-01-19 | 2012-07-18 | 合肥工业大学 | Niobate-based piezoelectric ceramic fiber/polymer 1-3 type composite material and preparation method |
| CN102491752B (en) * | 2011-11-18 | 2013-04-24 | 河南科技大学 | Preparation method of lithium and antimony doped potassium sodium niobate leadless piezoelectric ceramic |
| WO2013078993A1 (en) * | 2011-11-30 | 2013-06-06 | 深圳市大富科技股份有限公司 | Method for manufacturing microwave dielectric ceramic material |
| WO2013091560A1 (en) * | 2011-12-22 | 2013-06-27 | 深圳市大富科技股份有限公司 | Method for manufacturing microwave dielectric ceramic material |
| JP6457415B2 (en) | 2016-03-10 | 2019-01-23 | 太陽誘電株式会社 | Piezoelectric element and manufacturing method thereof |
| JP2018160535A (en) * | 2017-03-22 | 2018-10-11 | セイコーエプソン株式会社 | Piezoelectric element and piezoelectric element application device |
| CN108689711A (en) * | 2018-06-13 | 2018-10-23 | 合肥工业大学 | A kind of thermostable type sodium niobate based leadless piezoelectric ceramics and preparation method thereof |
| CN109650885B (en) * | 2018-12-11 | 2022-02-08 | 中国科学院上海硅酸盐研究所 | Lanthanum-doped silver niobate lead-free antiferroelectric energy storage ceramic material and preparation method thereof |
| CN110128139A (en) * | 2019-06-19 | 2019-08-16 | 哈尔滨理工大学 | A kind of KNN base ceramics and preparation method thereof with high-voltage electricity and high ferroelectric properties |
| CN110642622B (en) * | 2019-10-24 | 2021-09-24 | 桐乡清锋科技有限公司 | Potassium-sodium niobate-based leadless piezoelectric ceramic and manufacturing process and application thereof |
| CN113880575B (en) * | 2021-11-16 | 2023-03-21 | 江苏波速传感器有限公司 | Doped lead manganese niobate-lead zirconate titanate piezoelectric ceramic material and preparation method thereof |
| CN116813339B (en) * | 2023-05-12 | 2024-09-06 | 广东奥迪威传感科技股份有限公司 | Leadless piezoelectric ceramic and preparation method thereof |
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| CN101024573A (en) * | 2007-01-30 | 2007-08-29 | 合肥工业大学 | Multi-element sodium-potassium niobate series lead-free piezoelectric ceramic and preparing method |
| CN101037332A (en) * | 2007-04-20 | 2007-09-19 | 四川大学 | Multi constituent niobate lead-free piezoelectric ceramics |
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| CN101037332A (en) * | 2007-04-20 | 2007-09-19 | 四川大学 | Multi constituent niobate lead-free piezoelectric ceramics |
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