CN108275999A - A kind of preparation method of potassium niobate sodium-based leadless piezoelectric ceramic - Google Patents

A kind of preparation method of potassium niobate sodium-based leadless piezoelectric ceramic Download PDF

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CN108275999A
CN108275999A CN201810283072.XA CN201810283072A CN108275999A CN 108275999 A CN108275999 A CN 108275999A CN 201810283072 A CN201810283072 A CN 201810283072A CN 108275999 A CN108275999 A CN 108275999A
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杜毅
刘洋
孙晓
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Qilu University of Technology
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Abstract

The present invention relates to a kind of preparation method of potassium niobate sodium-based leadless piezoelectric ceramic, which is expressed as at being grouped as available chemical formula：(1‑x)(K0.5Na0.5)NbO3‑x(Bi0.5K0.5)ZrO3, wherein 0.02≤x≤0.06, the preparation method comprises the following steps：(1) weighing, dispensing, ball milling；(2) by tabletting after powder pre-burning；(3) it is sintered after potsherd dumping.Stringent control heating rate and sintering temperature obtain novel lead-free piezoceramic material by improving pre-burning and sintering temperature curve, sintering processing, and consistency promotes 10% or more compared with conventional sintering technique, piezoelectric coefficient d33Promote 50% or more.

Description

A kind of preparation method of potassium niobate sodium-based leadless piezoelectric ceramic
Technical field
The invention belongs to a kind of preparation methods of potassium niobate sodium-based leadless piezoelectric ceramic, belong to novel lead-free base function ceramics neck Domain.
Invention content
In order to solve the deficiencies in the prior art, the purpose of the present invention is to provide a kind of preparations of potassium-sodium niobate lead-free piezoelectric ceramics A kind of method, it is desirable to provide new ceramic green sintering method is effectively improved the sintering character and piezoelectric property of KNN ceramics.
In order to achieve the above technical purposes, the technical scheme is that：
A kind of preparation method of potassium sodium niobate piezoelectric ceramics of the present invention, it includes K mainly to prepare raw material2CO3、Na2CO3、 Nb2O5、Bi2O3、ZrO2.The ceramics are expressed as at being grouped as available chemical formula：(1-x)(K0.5Na0.5)NbO3-x(Bi0.5K0.5) ZrO3.It is characterized in that, the preparation method comprises the following steps：
(1) by raw material according to chemical formula (1-x) (K0.5Na0.5)NbO3-x(Bi0.5K0.5)ZrO3Proportioning weighed, dispensing.
(2) powder for obtaining step (1) is packed into agate jar, and agate ball is added, using absolute ethyl alcohol as ball-milling medium, Ball milling 20 hours, wherein raw material：Ballstone：Ethyl alcohol=1：2：1.5,300 mesh sieve is crossed after discharging drying, can get good fluidity Mixed powder.
(3) it by after pre-burning at 850 DEG C of mixed powder in step (2), is put into corundum crucible, it is small in 850 DEG C of pre-burnings 2 When, calcined temperature curve is：30 DEG C -500 DEG C keep the temperature 2 hours（1.5 DEG C/min of heating rate）- 850 DEG C keep the temperature 2 hours（It rises 3 DEG C/min of warm rate）- with stove natural cooling.It uses 5% polyvinyl alcohol to be ground as binder to powder is made, is granulated After sieve with 100 mesh sieve, the pressurize 30s under the pressure of 10MPa, pass through compression molding compacting needed for size potsherd.
(4) it by after the potsherd dumping in step (3), is sintered in Muffle furnace at 1050 DEG C after being buried with same component materials envelope 2 hours, sintering temperature curve was：30 DEG C -850 DEG C keep the temperature 2 hours（3 DEG C/min of heating rate）- 1050 DEG C keep the temperature 2 hours （1.5 DEG C/min of heating rate）- with stove natural cooling, leadless piezoelectric ceramics sample is finally made.
The study found that the consistency of potsherd has a significant impact to the sintering characteristic and electrical property of KNN leadless piezoelectric ceramics, The very high pottery of consistency can be made by improving calcining system curve, sintering processing in technical solution more than present invention use Tile.
Beneficial effects of the present invention：
(1) KNN potsherds consistency made from the preparation method of lead-free piezoelectric ceramic powder through the invention 93% with On, improve 10% or more compared to conventional sintering technique consistency.
(2) the KNN based leadless piezoelectric ceramics prepared through the invention have good electrical property, piezoelectric constant d33= 172pC/N；Electromechanical coupling factor kp=27.3%；Permittivity εr=370, dielectric loss tan δ=6.3%.
Description of the drawings
The present invention is further elaborated with reference to the accompanying drawings and detailed description：
Fig. 1 (1-x) (K0.5Na0.5)NbO3-x(Bi0.5K0.5)ZrO3The sintering schematic diagram of system ceramics sample（1 is the big earthenware of corundum Crucible, 2 for component powder, 3 be corundum small crucible with ceramic body, 4 be ceramic green, 5 be corundum plate）
Fig. 2 (1-x) (K0.5Na0.5)NbO3-x(Bi0.5K0.5)ZrO3The XRD diagram of system ceramics sample.
Specific implementation mode
A kind of preparation method of potassium niobate sodium-based leadless piezoelectric ceramic, includes the following steps：
Embodiment 1
(1) by raw material according to 0.98 (K of chemical formula0.5Na0.5)NbO3-0.02(Bi0.5K0.5)ZrO3Proportioning weighed, matched Material.
(2) powder for obtaining step (1) is packed into agate jar, and agate ball is added, using absolute ethyl alcohol as ball-milling medium, Ball milling 20 hours, wherein raw material：Ballstone：Ethyl alcohol=1：2：1.5,300 mesh sieve is crossed after discharging drying, can get good fluidity Mixed powder.
(3) it by after pre-burning at 850 DEG C of mixed powder in step (2), is put into corundum crucible, it is small in 850 DEG C of pre-burnings 2 When, calcined temperature curve is：30 DEG C -500 DEG C keep the temperature 2 hours（1.5 DEG C/min of heating rate）- 850 DEG C keep the temperature 2 hours（It rises 3 DEG C/min of warm rate）- with stove natural cooling.It uses 5% polyvinyl alcohol to be ground as binder to powder is made, is granulated After sieve with 100 mesh sieve, the pressurize 30s under the pressure of 10MPa, pass through compression molding compacting needed for size potsherd.
(4) it by after the potsherd dumping in step (3), is sintered in Muffle furnace at 1050 DEG C after being buried with same component materials envelope 2 hours, sintering temperature curve was：30 DEG C -850 DEG C keep the temperature 2 hours（3 DEG C/min of heating rate）- 1050 DEG C keep the temperature 2 hours （1.5 DEG C/min of heating rate）- with stove natural cooling, leadless piezoelectric ceramics sample is finally made；In the coating silver in potsherd two sides The after-applied 30 kV/cm DC voltages of electrode, polarize in 120 DEG C of silicone oil, and standing tests its electric property afterwards for 24 hours.Its electricity Performance d33=170pC/N；kp=26.2%；εr=369, tan δ=6.5%.
Embodiment 2
(1) by raw material according to 0.96 (K of chemical formula0.5Na0.5)NbO3-0.04(Bi0.5K0.5)ZrO3Proportioning weighed, matched Material.
(2) powder for obtaining step (1) is packed into agate jar, and agate ball is added, using absolute ethyl alcohol as ball-milling medium, Ball milling 20 hours, wherein raw material：Ballstone：Ethyl alcohol=1：2：1.5,300 mesh sieve is crossed after discharging drying, can get good fluidity Mixed powder.
(3) it by after pre-burning at 850 DEG C of mixed powder in step (2), is put into corundum crucible, it is small in 850 DEG C of pre-burnings 2 When, calcined temperature curve is：30 DEG C -500 DEG C keep the temperature 2 hours（1.5 DEG C/min of heating rate）- 850 DEG C keep the temperature 2 hours（It rises 3 DEG C/min of warm rate）- with stove natural cooling.It uses 5% polyvinyl alcohol to be ground as binder to powder is made, is granulated After sieve with 100 mesh sieve, the pressurize 30s under the pressure of 10MPa, pass through compression molding compacting needed for size potsherd.
(4) it by after the potsherd dumping in step (3), is sintered in Muffle furnace at 1050 DEG C after being buried with same component materials envelope 2 hours, sintering temperature curve was：30 DEG C -850 DEG C keep the temperature 2 hours（3 DEG C/min of heating rate）- 1050 DEG C keep the temperature 2 hours （1.5 DEG C/min of heating rate）- with stove natural cooling, leadless piezoelectric ceramics sample is finally made；In the coating silver in potsherd two sides The after-applied 30 kV/cm DC voltages of electrode, polarize in 120 DEG C of silicone oil, and standing tests its electric property afterwards for 24 hours.Its electricity Performance d33=172pC/N；kp=28.2%；εr=380, tan δ=6.6%.
Embodiment 3
(1) by raw material according to 0.94 (K of chemical formula0.5Na0.5)NbO3-0.06(Bi0.5K0.5)ZrO3Proportioning weighed, matched Material.
(2) powder for obtaining step (1) is packed into agate jar, and agate ball is added, using absolute ethyl alcohol as ball-milling medium, Ball milling 20 hours, wherein raw material：Ballstone：Ethyl alcohol=1：2：1.5,300 mesh sieve is crossed after discharging drying, can get good fluidity Mixed powder.
(3) it by after pre-burning at 850 DEG C of mixed powder in step (2), is put into corundum crucible, it is small in 850 DEG C of pre-burnings 2 When, calcined temperature curve is：30 DEG C -500 DEG C keep the temperature 2 hours（1.5 DEG C/min of heating rate）- 850 DEG C keep the temperature 2 hours（It rises 3 DEG C/min of warm rate）- with stove natural cooling.It uses 5% polyvinyl alcohol to be ground as binder to powder is made, is granulated After sieve with 100 mesh sieve, the pressurize 30s under the pressure of 10MPa, pass through compression molding compacting needed for size potsherd.
(4) it by after the potsherd dumping in step (3), is sintered in Muffle furnace at 1050 DEG C after being buried with same component materials envelope 2 hours, sintering temperature curve was：30 DEG C -850 DEG C keep the temperature 2 hours（3 DEG C/min of heating rate）- 1050 DEG C keep the temperature 2 hours （1.5 DEG C/min of heating rate）- with stove natural cooling, leadless piezoelectric ceramics sample is finally made；In the coating silver in potsherd two sides The after-applied 30 kV/cm DC voltages of electrode, polarize in 120 DEG C of silicone oil, and standing tests its electric property afterwards for 24 hours.Its electricity Performance d33=165pC/N；kp=27.3%；εr=370, tan δ=6.3%.

Claims (2)

1. a kind of preparation method of potassium sodium niobate piezoelectric ceramics, which is expressed as at being grouped as available chemical formula：(1-x) (K0.5Na0.5)NbO3-x(Bi0.5K0.5)ZrO3, it includes K mainly to prepare raw material2CO3、Na2CO3、Nb2O5、Bi2O3、ZrO2.It is special Sign is that the preparation method comprises the following steps：
(1) by raw material according to chemical formula (1-x) (K0.5Na0.5)NbO3-x(Bi0.5K0.5)ZrO3Proportioning weighed, dispensing and Ball milling can get uniform mixed powder.
(2) after the powder pre-burning for obtaining step (1), polyvinyl alcohol is added and is ground as binder to powder is made, makes The potsherd of size needed for compression molding compacting after grain.
(3) it by after the potsherd dumping in step (2), is buried in rear Muffle furnace and is sintered with same component materials envelope, be finally made unleaded Piezoelectric ceramics sample.
2. the preparation method of potassium niobate sodium-based leadless piezoelectric ceramic according to claim 1, it is characterised in that：Step (2) Middle material is put into corundum crucible, and in 850 DEG C of pre-burnings 2 hours, calcined temperature curve was：30 DEG C -500 DEG C keep the temperature 2 hours（It rises 1.5 DEG C/min of warm rate）- 850 DEG C keep the temperature 2 hours（3 DEG C/min of heating rate）- with stove natural cooling；It is ceramic in step (3) Piece is sintered 2 hours at 1050 DEG C in Muffle furnace, and sintering temperature curve is：30 DEG C -850 DEG C keep the temperature 2 hours（Heating rate 3 ℃/min）- 1050 DEG C keep the temperature 2 hours（1.5 DEG C/min of heating rate）- with stove natural cooling.
CN201810283072.XA 2018-04-02 2018-04-02 A kind of preparation method of potassium niobate sodium-based leadless piezoelectric ceramic Pending CN108275999A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110078505A (en) * 2019-05-17 2019-08-02 福州大学 A kind of high density KNN-BNN piezoelectric ceramics and its forming method
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
CN112234138A (en) * 2020-10-28 2021-01-15 中科传感技术(青岛)研究院 Preparation method of large-size multilayer piezoelectric ceramic
CN115093221A (en) * 2022-07-11 2022-09-23 广州凯立达电子股份有限公司 Potassium-sodium niobate-based leadless piezoelectric ceramic sheet, preparation method and application
CN116023138A (en) * 2022-12-22 2023-04-28 北京工业大学 Leadless piezoelectric ceramic material applied to energy collection in wide temperature range and preparation method thereof
CN116813336A (en) * 2023-06-30 2023-09-29 北京邮电大学 Method for optimizing PZT-based piezoelectric ceramic solid-phase sintering process

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KR101306419B1 (en) * 2011-10-07 2013-09-09 울산대학교 산학협력단 Electrostrictive Lead-free Ceramic Composition and Preparation Method Thereof
CN106278259A (en) * 2016-07-25 2017-01-04 北京中科奥倍超声波技术研究院 A kind of potassium niobate sodium base leadless piezoelectric

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101306419B1 (en) * 2011-10-07 2013-09-09 울산대학교 산학협력단 Electrostrictive Lead-free Ceramic Composition and Preparation Method Thereof
CN106278259A (en) * 2016-07-25 2017-01-04 北京中科奥倍超声波技术研究院 A kind of potassium niobate sodium base leadless piezoelectric

Cited By (8)

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CN110078505A (en) * 2019-05-17 2019-08-02 福州大学 A kind of high density KNN-BNN piezoelectric ceramics and its forming method
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
CN112234138A (en) * 2020-10-28 2021-01-15 中科传感技术(青岛)研究院 Preparation method of large-size multilayer piezoelectric ceramic
CN112234138B (en) * 2020-10-28 2022-08-12 中科传感技术(青岛)研究院 Preparation method of large-size multilayer piezoelectric ceramic
CN115093221A (en) * 2022-07-11 2022-09-23 广州凯立达电子股份有限公司 Potassium-sodium niobate-based leadless piezoelectric ceramic sheet, preparation method and application
CN116023138A (en) * 2022-12-22 2023-04-28 北京工业大学 Leadless piezoelectric ceramic material applied to energy collection in wide temperature range and preparation method thereof
CN116023138B (en) * 2022-12-22 2023-10-27 北京工业大学 Leadless piezoelectric ceramic material applied to energy collection in wide temperature range and preparation method thereof
CN116813336A (en) * 2023-06-30 2023-09-29 北京邮电大学 Method for optimizing PZT-based piezoelectric ceramic solid-phase sintering process

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