CN105732032A - High-compactness potassium sodium lithium niobate-calcium sodium bismuth titanate binary system lead-free piezoelectric ceramic and preparation method thereof - Google Patents
High-compactness potassium sodium lithium niobate-calcium sodium bismuth titanate binary system lead-free piezoelectric ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-compactness Sb<5+>-doped KNN-based lead-free piezoelectric ceramic and a preparation method thereof. A chemical formula of the piezoelectric ceramic is (k0.48, Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5, Na0.5)ZrO3 (KNLSxN-CBNZ in short), wherein x is equal to 0.01, 0.03, 0.05-0.08, 0.10. The KNLSxN-CBNZ lead-free piezoelectric ceramic prepared by a conventional solid-phase sintering process has d33 which can be up to 267pC/N, kp which is 45.2%, Tc which can be up to 253 DEG C, and compactness which can be as high as 4.63g/cm<3>. Lead-free piezoelectric ceramic components designed by the preparation method are simple in processing process; compared with other KNN-based lead-free piezoelectric ceramics, the high compactness of the high-compactness Sb<5+>-doped KNN-based lead-free piezoelectric ceramic enables the high-compactness Sb<5+>-doped KNN-based lead-free piezoelectric ceramic to be applied to apparatuses such as a piezoelectric ignitor and a piezoelectric buzzer; and the high-compactness Sb<5+>-doped KNN-based lead-free piezoelectric ceramic is a feasible lead-free piezoelectric material which replaces lead-containing piezoelectric ceramic in practical application.
Description
Technical field
The present invention relates to a kind of leadless piezoelectric ceramics, especially relate to the niobium potassium antimonate sodium lithium-zirconium of a kind of high-compactness
Acid bismuth sodium calcium binary system leadless piezoelectric ceramics and preparation method thereof, belongs to perovskite structure environment compatibility piezoelectric ceramics
Field.
Background technology
Piezoelectric ceramics, as a kind of important functionality ceramic, is often used in sensor, driver, ultrasonic transduction
In the devices such as device, buzzer and ignition, play in commercial production and daily life to closing weight
The effect wanted.Containing lead piezoelectric ceramics, such as Pb (Zr, Ti) O3(being abbreviated as PZT) due to the piezoelectric property of its excellence,
Dominate the market of piezoelectric ceramics always.But due to too high lead tolerance (～60wt%), in the preparation of pottery,
Using, the processing procedure after even discarding bring irreversible baneful influence all can to human body and environment.Along with people
Environmental consciousness promote and society extensive concern, a lot of countries and regions have all been issued and implemented some decrees and have been limited
The use of the harmful substances such as lead processed, such as, European Union has passed through in 2003 " to be limited in electronic and electrical equipment use
The instruction of harmful substance " (RoHS)；Japan has passed through " home electronics absorption method "；China is in 2006 also
A series of regulations such as " electronics and IT products produce prevention and cure of pollution management method " are issued.Although by technical problem,
Some leaded piezo-electric devices temporarily have immunity, but just fail to these immunities of in July, 2016.
So the research of leadless piezoelectric ceramics is extremely urgent.
The research of leadless piezoelectric ceramics, main leadless piezoelectric ceramics currently mainly have BaTiO3-system, (K, Na)
NbO3-system, (Bi, Na) TiO3-system etc., and (K, Na) NbO3Pottery is because of its of a relatively high piezoelectricity
Coefficient and higher Curie temperature and obtained the biggest concern, particularly saito etc. are by template grain growth,
It is prepared for KNN-base piezoelectric ceramics coefficient d33After ≈ 416pC/N, start the research of KNN-base pottery further
Upsurge.In order to promote the performance of KNN-base piezoelectric ceramic, common research method has three kinds: nanometer farmland engineering,
Crystal grain method for alignment and phase boundary engineering.But from the point of view of KNN-base pottery, although much study at piezoelectric property
On obtain the biggest lifting, but owing to the consistency of pottery is relatively low, obtained the biggest limit in actual applications
System.In order to improve the consistency of pottery, existing frequently-used method mostly is special processing technique, such as: laser etc.
Gas ions sinters, hot pressed sintering etc..But these special processing technique, complex technical process, processing cost is high
Be not suitable for industrialized production.Build phase boundary by room temperature at present, base metal niobate based leadless piezoelectricity can be made to make pottery
The performance of porcelain is remarkably enhanced, and therefore, promotes piezoelectricity and the cause of base metal niobate leadless piezoelectric ceramics
Density becomes the principal direction of the research of potassium niobate sodium-based leadless piezoelectric ceramic application.
Summary of the invention
The purpose of the present invention is contemplated to prepare high tension electricity coefficient and high-compactness with traditional solid-phase sintering process
Potassium niobate sodium-based leadless piezoelectric ceramic, it is provided that the niobium potassium antimonate sodium lithium of a kind of high-compactness-zirconic acid bismuth sodium calcium binary system
Leadless piezoelectric ceramics.The method uses niobium potassium antimonate sodium lithium-zirconic acid bismuth sodium calcium binary prepared by conventional solid sintering process
Series lead-free piezoelectric ceramic, its consistency is up to 4.63g/cm3, piezoelectric constant d33For 267pC/N, planar electromechanical
Coefficient of coup kpUp to 45.2%, TcUp to 253 DEG C
The purpose of the present invention can be achieved through the following technical solutions:
The basic ideas of the present invention are: realize niobium potassium antimonate sodium lithium-zirconic acid bismuth by the design and optimization of phase structure
Sodium calcium binary system leadless piezoelectric ceramics high-compactness, the purpose of high tension performance, its concrete grammar is: add Sb
The high-T_c superconductors temperature of potassium-sodium niobate lithium-zirconic acid bismuth sodium calcium ceramic systems is being reduced, is promoting potassium niobate simultaneously
Tripartite-orthorhombic phase the temperature of sodium lithium-zirconic acid bismuth sodium calcium ceramic systems；Thus it is biphase at room temperature to form tripartite-four directions
The niobium potassium antimonate sodium lithium coexisted-zirconic acid bismuth sodium calcium binary system leadless piezoelectric ceramics, its formula is (k0.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3。
The niobium potassium antimonate sodium lithium of a kind of high-compactness of the present invention-zirconic acid bismuth sodium calcium binary system leadless piezoelectric pottery
Porcelain, by formula (k0.48,Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3Represent, the x generation in formula
The atomic number that in gauge pressure electroceramics system, Sb element is shared in constituent element, i.e. atomic percent, x=0.01 in formula, 0.03
0.05-0.08,0.10。
The niobium potassium antimonate sodium lithium of high-compactness of the present invention-zirconic acid bismuth sodium calcium binary system leadless piezoelectric ceramics, it is brilliant
Body structure is perovskite structure.
The niobium potassium antimonate sodium lithium of high-compactness of the present invention-zirconic acid bismuth sodium calcium binary system leadless piezoelectric ceramics, its
Consistency is up to 4.63g/cm3, piezoelectric constant d33For 267pC/N, planar electromechanical coupling factor kpUp to 45.2%,
TcUp to 253 DEG C.
The preparation of any of the above-described described niobium potassium antimonate sodium lithium-zirconic acid bismuth sodium calcium binary system leadless piezoelectric ceramics of the present invention
Method, comprises the following steps that:
(1) conventional solid sintering process method preparation technology is used, with analytically pure sodium carbonate, potassium carbonate, five oxygen
Changing two niobiums, antimony oxide, lithium carbonate, calcium carbonate, bismuth oxide, zirconium oxide is raw material, according to corresponding system
(k0.48,Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3Carry out dispensing, x=0.01 in formula, 0.03
0.05-0.08,0.10；
(2) raw material that step (1) is prepared with dehydrated alcohol as ball-milling medium, little with planetary ball mill 24
Time post-drying obtain mixed powder；
(3) step (2) gained mixed powder is incubated pre-burning in 6 hours at 850 DEG C, in pre-burned powder
Add the polyvinyl alcohol water solution pelletize of 5wt%；
(4) by powder good for step (3) pelletize, column type mould is utilized to be compressed into disc-shaped base substrate, and
After 450 DEG C of binder removals 3 hours, at 3 hours sintering of 1100-1120 DEG C of insulation, obtain potsherd, use Archimedes's draining
Method records the density of pottery；
(5) by upper silver electrode after the potsherd sand paper two sides that step (4) sinters being polished；Pottery by upper silver electrode
Sheet is in the silicone oil of 30 DEG C, and polarize under the voltage that electric field intensity is 3kV/mm 15min；
(6), after having polarized, described potsherd is taken out from silicone oil, i.e. obtain the niobium potassium antimonate sodium lithium of high-compactness-
Zirconic acid bismuth sodium calcium binary system leadless piezoelectric ceramics, after it is stood 24 hours in atmosphere, uses ieee standard
Measure the electric property of gained leadless piezoelectric ceramics.
The present invention has the following advantages and useful technique effect:
1, the leadless piezoelectric ceramics that the present invention provides has potassium niobate sodium base leadless prepared by conventional solid sintering method
The highest consistency of piezoelectric ceramics, its consistency is up to 4.63g/cm3, piezoelectric constant d33It is 267
PC/N, planar electromechanical coupling factor kpUp to 45.2%, TcUp to 253 DEG C.
2, the leadless piezoelectric ceramics that the present invention provides uses fine copper solid-phase sintering method to prepare, and puts a little than plasma
Sintering, the technique such as hot pressed sintering, low cost, preparation method is simple, has the operable of reality in the industrial production
Property.
3, the leadless piezoelectric ceramics that the present invention provides, piezoelectric property is excellent, can apply in piezoelectric buzzer and pressure
On electric igniter.
Accompanying drawing explanation
Fig. 1 is the (k when x=0.01,0.030.05,0.10 changes value prepared by embodiment 10.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The leadless piezoelectric ceramics relative Jie under 10kHz
Electric constant εrVariation with temperature curve；
Fig. 2 is the (k when x=0.01,0.030.05-0.08,0.10 changes value prepared by embodiment 10.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The x-ray diffraction collection of illustrative plates of leadless piezoelectric ceramics；
Fig. 3 is the (k when x=0.01,0.030.06,0.10 changes value prepared by embodiment 10.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The surface Scanning Electron of leadless piezoelectric ceramics is micro-
Picture；
Fig. 4 is the (k when x=0.01,0.030.06,0.10 changes value prepared by embodiment 10.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The ferroelectric hysteresis loop figure of leadless piezoelectric ceramics；
Fig. 5 is the (k when x=0.01,0.030.06,0.10 changes value prepared by embodiment 10.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3(a) density of leadless piezoelectric ceramics and Sb's
Graph of a relation and (b) sample photo；
Fig. 6 is the (k when x=0.01,0.030.06,0.10 changes value prepared by embodiment 10.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The d of leadless piezoelectric ceramics33And kpContain about Sb
The graph of a relation of amount.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail, and following example can make this specialty
Technical staff is more completely understood by the present invention, but limits the present invention never in any form, the knack people in this field
Member can make improvement and the adjustment of some non-intrinsically safes according to the content of foregoing invention.
Embodiment 1
According to formula (k0.48,Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The niobium potassium antimonate represented
Sodium lithium-zirconic acid bismuth sodium calcium binary system leadless piezoelectric ceramics content carries out dispensing.
As x=0.01, its formula is (k0.48,Na0.52)0.95Li0.05Nb0.99Sb0.01-0.03Ca0.5(Bi0.5,Na0.5)ZrO3
The first step: with analytically pure sodium carbonate, potassium carbonate, niobium pentaoxide, antimony oxide, lithium carbonate, carbon
Acid calcium, bismuth oxide, zirconium oxide is raw material, according to stoichiometric proportion, calculates required each powder quality and weighs,
Raw material；
Second step: the raw material that the first step is prepared with dehydrated alcohol as ball-milling medium, little with planetary ball mill 24
Time post-drying obtain mixed powder；
3rd step: second step gained mixed powder is incubated pre-burning in 6 hours at 850 DEG C, in pre-burned powder
Add the polyvinyl alcohol water solution pelletize of 5wt%；
4th step: by powder good for the 3rd step pelletize, utilizes column type mould to be compressed into disc-shaped base substrate, and
After 450 DEG C of binder removals 3 hours, at 3 hours sintering of 1120 DEG C of insulations, obtain potsherd, use Archimedes's drainage to survey
Obtain ceramic density；
5th step: the potsherd sand paper two sides that the 4th step is sintered polish after by upper silver electrode；Pottery by upper silver electrode
Ceramics is in the silicone oil of 30 DEG C, and polarize under the voltage that electric field intensity is 3kV/mm 15min；
6th step: after having polarized, takes out described potsherd from silicone oil, i.e. obtains the niobium potassium antimonate of high-compactness
Sodium lithium-zirconic acid bismuth sodium calcium binary system leadless piezoelectric ceramics, after it is stood 24 hours in atmosphere, uses IEEE
The consistency of canonical measure this leadless piezoelectric ceramics of gained and electric property.
Ceramic dense degree: ρ=4.46g/cm3；
Pottery electric property: d33=87pC/N, kp=20.8%, εr=948, Tc=363 DEG C.
Embodiment 2
As x=0.03, its formula is (k0.48,Na0.52)0.95Li0.05Nb0.97Sb0.03-0.03Ca0.5(Bi0.5,Na0.5)ZrO3
Preparation method in the present embodiment is same as in Example 1, differs only in preparation process sintering condition not
With, the sintering temperature of this example is 1116 DEG C.
Ceramic dense degree: ρ=4.40g/cm3；
Pottery electric property: d33=163pC/N, kp=18.4%, εr=1145, Tc=314 DEG C.
Embodiment 3
As x=0.05, its formula is (k0.48,Na0.52)0.95Li0.05Nb0.95Sb0.05-0.03Ca0.5(Bi0.5,Na0.5)ZrO3
Preparation method in the present embodiment is same as in Example 1, differs only in preparation process sintering condition not
With, the sintering temperature of this example is 1112 DEG C.
Ceramic dense degree: ρ=4.56g/cm3；
Pottery electric property: d33=217pC/N, kp=32.3%, εr=1836, Tc=280 DEG C.
Embodiment 4
As x=0.06, its formula is (k0.48,Na0.52)0.95Li0.05Nb0.94Sb0.06-0.03Ca0.5(Bi0.5,Na0.5)ZrO3
Preparation method in the present embodiment is same as in Example 1, differs only in preparation process sintering condition not
With, the sintering temperature of this example is 1110 DEG C.
Ceramic dense degree: ρ=4.63g/cm3；
Pottery electric property: d33=267pC/N, kp=45.2%, εr=1836, Tc=253 DEG C.
Embodiment 5
As x=0.07, its formula is (k0.48,Na0.52)0.95Li0.05Nb0.93Sb0.07-0.03Ca0.5(Bi0.5,Na0.5)ZrO3
Preparation method in the present embodiment is same as in Example 1, differs only in preparation process sintering condition not
With, the sintering temperature of this example is 1108 DEG C.
Ceramic dense degree: ρ=4.68g/cm3；
Pottery electric property: d33=225pC/N, kp=39.3%, εr=1892, Tc=220 DEG C.
Embodiment 6
As x=0.08, its formula is (k0.48,Na0.52)0.95Li0.05Nb0.92Sb0.08-0.03Ca0.5(Bi0.5,Na0.5)ZrO3
Preparation method in the present embodiment is same as in Example 1, differs only in preparation process sintering condition not
With, the sintering temperature of this example is 1106 DEG C.
Ceramic dense degree: ρ=4.65g/cm3；
Pottery electric property: d33=220pC/N, kp=37.2%, εr=2091, Tc=206 DEG C.
Embodiment 7
As x=0.10, its formula is (k0.48,Na0.52)0.95Li0.05Nb0.90Sb0.10-0.03Ca0.5(Bi0.5,Na0.5)ZrO3
Preparation method in the present embodiment is same as in Example 1, differs only in preparation process sintering condition not
With, the sintering temperature of this example is 1100 DEG C.
Ceramic dense degree: ρ=4.62g/cm3；
Pottery electric property: d33=180pC/N, kp=22.1%, εr=2941, Tc=152 DEG C.
Fig. 1 is the (k when x=0.01,0.06,0.08,0.10 changes value prepared by the present invention0.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The leadless piezoelectric ceramics relative Jie under 10kHz
Electric constant εrVariation with temperature curve, it can be seen that the change of phase transition temperature: when under x=0.01 room temperature
It is orthogonal-four directions coexisting phase, when 0.06≤x≤0.10, is tripartite-four directions coexisting phase under room temperature.
Fig. 2 is (k when x=0.01,0.030.05-0.08,0.10 changes value0.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The x-ray diffraction collection of illustrative plates of leadless piezoelectric ceramics,
It appeared that all of pottery prepared by the present invention is at room temperature perovskite structure from figure.Inserting on the right side of chart
The Lorentz fit peak of diffraction maximum when figure is 2 θ=44.5-46.5 °, when as can be seen from the figure when x≤0.03, matching
Four peaks are gone out, the peak (pink) (200) of the most corresponding two TetragonalsT(002)TAnd the peak of two orthorhombic phase is (purple
Color) (020)O(200)O/(002)O.As x=0.05, two peaks and Tetragonal (pink) (200) are simulatedTWith
(002)TPeak position the most corresponding, and the strong ratio in the peak at two peaks is 2:1.When 0.06≤x≤0.10, three Lorentz peaks
Represent two Tetragonals (pink) (200) respectivelyT(002)TPeak (crocus) (002) with tripartite's phaseR。
It can be seen that under room temperature, when Sb content x≤0.03, ceramic systems is O-T two-phase coexistent, along with Sb content
Increase and become R-T two-phase coexistent phase from Tetragonal, during Zhongdao x=0.10, become the R-T two-phase coexistent phase of suppression.
Fig. 3 is the prepared (k when x=0.01,0.03 0.06,0.10 changes value0.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The surface Scanning Electron of leadless piezoelectric ceramics is micro-
Picture；Figure can be seen that, crystallite dimension has the sensitiveest change to Sb content.Crystal grain in all of component is all
Showing as CRYSTALLITE SIZES bivariate distribution, this is one of ceramic reason obtaining higher-density.Along with Sb content
Increase, ceramic crystalline grain is at x > 0.03 time crystallite dimension start to be obviously reduced, as x=0.10, crystallite dimension is significant
Diminish, and more they tend to homogenization.
Fig. 4 is the prepared (k when x=0.01,0.03 0.06,0.10 changes value0.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The ferroelectric hysteresis loop figure of leadless piezoelectric ceramics.All
The ferroelectric hysteresis loop of component is all typical P-E ring structure, and the ferroelectric properties of material and Sb content have the biggest
Relation.As can be seen from the figure PrAlong with the increase ascendant trend before this of Sb content, begin to decline when x >=0.06,
And EcThe increase being then as Sb content presents a general trend declined.
Fig. 5 is the prepared (k when x=0.01,0.03 0.06,0.10 changes value0.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3(a) density of leadless piezoelectric ceramics and Sb's
Graph of a relation and (b) sample photo, it can be seen that in the range of 0.06≤x≤0.08, pottery has the highest
Consistency (4.63-4.68g/cm3) this and microstructural compactness is closely bound up, this scope is also and pottery simultaneously
The R-T phase boundary of porcelain keeps consistent.Figure gives the photo of sintering pottery simultaneously, it can be seen that make pottery in total figure
Porcelain presents good sintering character.
Fig. 6 is the prepared (k when x=0.01,0.03 0.06,0.10 changes value0.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3The d of leadless piezoelectric ceramics33And kpContain about Sb
The graph of a relation of amount, d33Obtained maximum 267pC/N when x=0.06, the increase then as Sb content is opened
Begin to reduce.It should be noted that d33In a bigger Sb content range, (0.06≤x≤0.08) also keeps
One bigger value (220-267pC/N).The more important thing is kpVariation tendency and d33Keep consistent.
Although the preferred embodiments of the present invention being described above in conjunction with accompanying drawing, but the invention is not limited in
Above-mentioned detailed description of the invention, above-mentioned detailed description of the invention is only schematically, is not restrictive, ability
The those of ordinary skill in territory is under the enlightenment of the present invention, without departing from present inventive concept and claimed model
In the case of enclosing, it is also possible to make the concrete conversion of a lot of form, within these belong to protection scope of the present invention.
Claims (7)
1. the niobium potassium antimonate sodium lithium of high-compactness-zirconic acid bismuth sodium calcium binary system leadless piezoelectric ceramics, its feature exists
In, this binary system leadless piezoelectric ceramics is by formula (k0.48,
Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3Representing, the x in formula represents in piezoelectric ceramics system
The atomic number that Sb element is shared in constituent element, i.e. atomic percent, x=0.01 in formula, 0.03,0.05-0.08 or 0.10.
The niobium potassium antimonate sodium lithium of high-compactness the most according to claim 1-zirconic acid bismuth sodium unleaded pressure of calcium binary system
Electroceramics, it is characterised in that the crystal structure of described binary system leadless piezoelectric ceramics is perovskite structure.
The niobium potassium antimonate sodium lithium of high-compactness the most according to claim 1 and 2-zirconic acid bismuth sodium calcium binary system without
Lead piezoelectric ceramics, it is characterised in that the consistency of described binary system leadless piezoelectric ceramics is up to 4.63g/cm3,
Piezoelectric constant d33For 267pC/N, planar electromechanical coupling factor kpReach 45.2%, TcUp to 253 DEG C.
4. the niobium potassium antimonate sodium lithium of a high-compactness as claimed in claim 1 or 2-zirconic acid bismuth sodium calcium binary system
The preparation method of leadless piezoelectric ceramics, it is characterised in that comprise the following steps that:
(1) conventional solid sintering process method preparation technology is used, with analytically pure sodium carbonate, potassium carbonate, five oxygen
Changing two niobiums, antimony oxide, lithium carbonate, calcium carbonate, bismuth oxide, zirconium oxide is raw material, according to corresponding system
(k0.48,Na0.52)0.95Li0.05Nb1-xSbx-0.03Ca0.5(Bi0.5,Na0.5)ZrO3Carry out dispensing；
(2) the raw material planetary ball mill post-drying that step (1) prepares is obtained mixed powder；
(3) step (2) gained mixed powder is incubated pre-burning in 6 hours at 850 DEG C, in pre-burned powder
Add the polyvinyl alcohol water solution pelletize of 5wt%；
(4) by powder good for step (3) pelletize, it is pressed into disc-shaped base substrate, and 450 DEG C of binder removals 3 hours
After, at 3 hours sintering of 1100-1120 DEG C of insulation, obtain potsherd；
(5) by upper silver electrode after the potsherd two sides that step (4) sinters being polished；Existed by the potsherd of upper silver electrode
In the silicone oil of 30 DEG C, polarize under the voltage that electric field intensity is 3kV/mm 15min, takes out the niobium i.e. obtaining high-compactness
Potassium antimonate sodium lithium-zirconic acid bismuth sodium calcium binary system leadless piezoelectric ceramics.
The niobium potassium antimonate sodium lithium of high-compactness the most according to claim 4-zirconic acid bismuth sodium unleaded pressure of calcium binary system
The preparation method of electroceramics, it is characterised in that the medium that the planetary ball mill described in step (2) uses is anhydrous second
Alcohol, Ball-milling Time is 24h.
The niobium potassium antimonate sodium lithium of high-compactness the most according to claim 4-zirconic acid bismuth sodium unleaded pressure of calcium binary system
The preparation method of electroceramics, it is characterised in that step (4) described potsherd uses Archimedes's drainage to record pottery
The density of porcelain.
The niobium potassium antimonate sodium lithium of high-compactness the most according to claim 4-zirconic acid bismuth sodium unleaded pressure of calcium binary system
The preparation method of electroceramics, it is characterised in that the niobium potassium antimonate sodium lithium of described high-compactness-zirconic acid bismuth sodium calcium two
After unit's series lead-free piezoelectric ceramic stands 24 hours in atmosphere, ieee standard is used to measure its electric property.
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