CN106187182A - The preparation method of PZT base piezoelectric ceramic - Google Patents

The preparation method of PZT base piezoelectric ceramic Download PDF

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CN106187182A
CN106187182A CN201610582999.4A CN201610582999A CN106187182A CN 106187182 A CN106187182 A CN 106187182A CN 201610582999 A CN201610582999 A CN 201610582999A CN 106187182 A CN106187182 A CN 106187182A
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powder
pzt
preparation
mno
slurry
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刘洁
王竹
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ANHUI HUASEN PAPER Co Ltd
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ANHUI HUASEN PAPER Co Ltd
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
    • C04B35/491—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
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Abstract

The present invention relates to the preparation method of PZT base piezoelectric ceramic, can effectively solve the problem that piezoelectric constant is low, temperature stability is poor and service life is short of PZT pottery, method is, by PZT powder and MnO2Powder mixes, and adds water, ball milling, form slurry, dries, and adds binding agent, become blank, compressing, plastic removal, sintering, obtain piezoelectric ceramics, polishing, coat silver slurry, form silver electrode on two surfaces, be then placed in silicone oil, electric field polarization 5 60min, PZT base piezoelectric ceramic.Abundant raw material of the present invention, scientific formula, preparation method is simple, and excellent product performance improves piezoelectric parameter, and service life is long, is that on piezoceramic material innovates greatly.

Description

The preparation method of PZT base piezoelectric ceramic
Technical field
The present invention relates to electromechanical equipment material, the preparation method of a kind of PZT base piezoelectric ceramic.
Background technology
Piezoelectric ceramics can realize the mutual conversion between mechanical energy and electric energy, utilizes the electromechanical equipment that piezoelectric ceramics is made As sensor, transducer etc. have been widely used in military affairs, national defence, medical treatment and the every field of human being's production life. PZT base piezoelectric ceramic since find since due to the electric property of its excellence be a most widely used general class ceramic material.At present, exist The PZT base pottery of the mainly Mn-modified used in power-type ultrasonic transducer, this kind of piezoelectric ceramics strain constant d33On the low side Only have 230-330pC/N, have a strong impact on the conversion efficiency between electric energy and mechanical energy, the additionally temperature stability of such material Difference, causes transducer to be not suitable in high temperature environments using and service life is short, it is impossible to meets power ultrasonic and wants device Ask, finally have impact on the development in power ultrasonic field.Therefore, in order to solve, piezoelectric ceramics performance is low, temperature stability is poor, use The problems such as the life-span is short, need to develop the PZT base piezoelectric ceramic of a kind of high tension performance high-temperature stability so that it is can disclosure satisfy that The requirement in power ultrasonic field at present, thus promote the development of power ultrasonic.
Summary of the invention
For above-mentioned situation, for overcoming the defect of prior art, the purpose of the present invention is just to provide a kind of PZT base piezoelectricity pottery The preparation method of porcelain, can effectively solve the problem that piezoelectric constant is low, temperature stability is poor and service life is short of PZT pottery.
The technical scheme that the present invention solves is to be realized by following steps:
(1) by PZT powder and MnO2Powder mixes, and becomes mixed-powder, MnO2Powder with PZT powder quality ratio is (0.001 ~ 0.70) 1；
(2) add water form slurry by mixed-powder, and ball milling 1-72h makes the slurry that powder body mix homogeneously, granular size are consistent；
(3) slurry is dried, add the binding agent of siccative weight 1-10%, become blank；
(4) compressing, it is that 200-330MPa carries out ceramic blank molding to blank at pressure；
(5) ceramic blank that step (4) is made is put into plastic removal in Muffle furnace, plastic removal temperature 500-800 DEG C, plastic removal time 1-5h, Become preform；
(6) preform being put in Muffle furnace and sinter, sintering temperature is 1200-1300 DEG C, and sintering time 1-5h obtains piezoelectric ceramics (also known as PZT:xMnO2Piezoelectric ceramics,xFor MnO2With the mass content ratio of PZT, in the present inventionxIt is 0.001 ~ 0.70, i.e. 0.001 ~ 0.70 1)；
(7), after the upper and lower surface of pottery step (6) obtained is polished, repaste silver slurry, calcine 10-at 550-750 DEG C 60min, forms silver electrode on two surfaces；
(8) piezoelectric ceramics having silver electrode is placed in silicone oil, with the electric field polarization 5-60min of 3-5kV/mm, PZT base pressure Electroceramics.
Abundant raw material of the present invention, scientific formula, preparation method is simple, and excellent product performance improves piezoelectric parameter, uses Life-span is long, is that on piezoceramic material innovates greatly.
Detailed description of the invention
Below in conjunction with embodiment, the detailed description of the invention of the present invention is elaborated.
The present invention can be given by following example in being embodied as.
Embodiment 1
The present invention, in being embodied as, can be realized by following steps:
(1) by PZT powder and MnO2Powder mixes, and becomes mixed-powder, MnO2Powder with PZT powder quality ratio is 0.05 1；
(2) add water form slurry by mixed-powder, loads in planetary ball mill, and ball milling 12h makes powder body mix homogeneously, granule big Little consistent slurry；
(3) slurry is dried, add the binding agent of siccative weight 3-10%, place 24h, become blank；
(4) compressing, it is that 250MPa carries out ceramic blank molding, blank diameter 25mm to blank at pressure；
(5) ceramic blank that step (4) is made is put into corundum crucible, be then placed in plastic removal in Muffle furnace, plastic removal temperature 600-700 DEG C, plastic removal time 2h, become preform；
(6) preform being put in Muffle furnace and sinter, sintering temperature is 1200-1290 DEG C, sintering time 4h, heating rate 1-4 DEG C/ Min, obtains piezoelectric ceramics；
(7), after the upper and lower surface of pottery step (6) obtained is polished, repaste silver slurry, calcine 30min at 550 DEG C, Two surfaces form the silver electrode of 30 microns；
(8) piezoelectric ceramics having silver electrode is placed in silicone oil, with the electric field polarization 15min of 3.5kV/mm, PZT base piezoelectricity Pottery is (also known as PZT 0.05MnO2Piezoelectric ceramics).
The present invention in force, also can be given by following example.
Embodiment 2
The present invention in being embodied as, described MnO2Powder is 0.075 1 with PZT powder quality ratio.
Embodiment 3
The present invention in being embodied as, described MnO2Powder is 0.1 1 with PZT powder quality ratio.
Embodiment 4
The present invention in being embodied as, described MnO2Powder is 0.15 1 with PZT powder quality ratio.
Embodiment 5
The present invention in being embodied as, described MnO2Powder is 0.2 1 with PZT powder quality ratio.
Embodiment 6
The present invention in being embodied as, described MnO2Powder is 0.25 1 with PZT powder quality ratio.
The preparation method of embodiment 2-6 is by embodiment 1.
The present invention applies on the spot and tests, and the piezoelectric constant of PZT pottery improves more than 30%, and 200 DEG C of annealing Process the piezoelectric constant of 100h stably rear pottery > 340pC/N, it was demonstrated that PZT pottery can work long hours at 200 DEG C, extends Service life, and the piezoelectric constant ceramic with the power-type produced both at home and abroadd 33, planar electromechanical coupling factork p, mechanical quality because of NumberQ mContrast, there is obvious advantage, have significantly progressive, the relevant test case of embodiment 1-6 and relevant comparative are such as Following table:
Table 1
Ceramic composition d 33(pC/N) k p Q m
PZT-0.05MnO2 445 0.63 600 The present invention
PZT-0.75MnO2 455 0.61 500 The present invention
PZT-0.1MnO2 426 0.60 500 The present invention
PZT-0.15MnO2 403 0.58 500 The present invention
PZT-0.2MnO2 340 0.57 300 The present invention
PZT-0.25MnO2 313 0.56 300 The present invention
PZT 240-310 0.55-0.57 500-1000 Germany
PZT840 290 0.59 500 The U.S.
PZT8 230 0.53 800 China
PZT85 330 0.57 1800 China
Table 2
Pottery model Annealing temperature d 33(pC/N)
PZT-0.1MnO2 250 255
PZT85 250 120
PZT:0.1MnO after 250 DEG C of annealings in table 22Pottery and PZT85 potteryd 33Contrast, it can be seen that PZT: 0.1MnO2After pottery is returned goods at 250 DEG Cd 33It is 255 pC/N, higher than traditional PZT8 pottery, illustrates that the pottery of the present invention can To use in high temperature environments.
By upper it should be apparent that the piezoelectric constant of PZT pottery improves more than 30%, and 200 DEG C of annealings The piezoelectric constant of 100h stably rear pottery > 340pC/N, illustrate that pottery can work long hours at 200 ° of C, the PZT of the present invention:xMnO2Piezoelectric ceramics and traditional power-type PZT ceramic phase ratio, piezoelectric constant raising reaches 30%, and temperature stability has obtained the biggest Improvement, be more suitable in the hot environment of more than 200 DEG C use, solve current power-type ultrasonic transducer conversion efficiency The problem that low and operating temperature is low, economic and social benefit is huge.

Claims (7)

1. the preparation method of a PZT base piezoelectric ceramic, it is characterised in that realized by following steps:
(1) by PZT powder and MnO2Powder mixes, and becomes mixed-powder, MnO2Powder with PZT powder quality ratio is (0.001 ~ 0.70) 1；
(2) add water form slurry by mixed-powder, ball milling 1-72h, prepared powder body mix homogeneously, the slurry that granular size is consistent；
(3) slurry is dried, add the binding agent of siccative weight 1%-10%, become blank；
(4) compressing, under the conditions of pressure is 200-330MPa, blank is carried out ceramic blank molding；
(5) ceramic blank that step (4) is made is put into plastic removal in Muffle furnace, plastic removal temperature 500-800 DEG C, plastic removal time 1-5h, Become preform；
(6) preform being put in Muffle furnace and sinter, sintering temperature is 1200-1300 DEG C, sintering time 1-5h, obtains piezoelectricity pottery Porcelain；
(7), after the upper and lower surface of piezoelectric ceramics step (6) obtained is polished, silver slurry is repasted, 550-750 DEG C of calcining 10-60min, forms silver electrode on two surfaces；
(8) piezoelectric ceramics having silver electrode is placed in silicone oil, with the electric field polarization 5-60min of 3-5kV/mm, PZT base pressure Electroceramics.
The preparation method of PZT base piezoelectric ceramic the most according to claim 1, it is characterised in that realized by following steps:
(1) by PZT powder and MnO2Powder mixes, and becomes mixed-powder, MnO2Powder is 0.05 with PZT powder quality ratio 1；
(2) add water form slurry by mixed-powder, loads in planetary ball mill, and ball milling 12h prepares powder body mix homogeneously, granule Slurry of the same size；
(3) slurry is dried, add the binding agent of siccative weight 3%-10%, place 24h, become blank；
(4) compressing, under the conditions of pressure is 250MPa, blank is carried out ceramic blank molding, blank diameter 25mm；
(5) ceramic blank that step (4) is made is put into corundum crucible, be then placed in plastic removal in Muffle furnace, plastic removal temperature 600-700 DEG C, plastic removal time 2h, become preform；
(6) preform being put in Muffle furnace and sinter, sintering temperature is 1200-1290 DEG C, sintering time 4h, heating rate 1-4 DEG C/ Min, obtains piezoelectric ceramics；
(7), after the upper and lower surface of pottery step (6) obtained is polished, repaste silver slurry, calcine 30min at 550 DEG C, Two surfaces form the silver electrode of 30 microns；
(8) piezoelectric ceramics having silver electrode is placed in silicone oil, with the electric field polarization 15min of 3.5kV/mm, PZT base piezoelectricity Pottery.
The preparation method of PZT base piezoelectric ceramic the most according to claim 1, it is characterised in that described MnO2Powder with PZT powder quality ratio is 0.075 1.
The preparation method of PZT base piezoelectric ceramic the most according to claim 1, it is characterised in that described MnO2Powder with PZT powder quality ratio is 0.1 1.
The preparation method of PZT base piezoelectric ceramic the most according to claim 1, it is characterised in that described MnO2Powder with PZT powder quality ratio is 0.15 1.
The preparation method of PZT base piezoelectric ceramic the most according to claim 1, it is characterised in that described MnO2Powder with PZT powder quality ratio is 0.2 1.
The preparation method of PZT base piezoelectric ceramic the most according to claim 1, it is characterised in that described MnO2Powder with PZT powder quality ratio is 0.25 1.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108046801A (en) * 2017-11-20 2018-05-18 沧州奥力威智能科技有限公司 Piezoelectric ceramic composition and preparation method thereof
CN114835489A (en) * 2022-05-11 2022-08-02 国网智能电网研究院有限公司 Potassium-sodium niobate-based leadless piezoelectric ceramic and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104291817A (en) * 2013-07-17 2015-01-21 淄博宇海电子陶瓷有限公司 High-Curie-temperature PZT piezoceramic material and preparation method thereof
CN104810472A (en) * 2015-04-10 2015-07-29 北京大学 Piezoelectric ceramic with piezoelectric coefficient of d36 and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104291817A (en) * 2013-07-17 2015-01-21 淄博宇海电子陶瓷有限公司 High-Curie-temperature PZT piezoceramic material and preparation method thereof
CN104810472A (en) * 2015-04-10 2015-07-29 北京大学 Piezoelectric ceramic with piezoelectric coefficient of d36 and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈治清: "《口腔生物材料学》", 30 June 2004 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108046801A (en) * 2017-11-20 2018-05-18 沧州奥力威智能科技有限公司 Piezoelectric ceramic composition and preparation method thereof
CN108046801B (en) * 2017-11-20 2021-07-06 蔡豪杰 Piezoelectric ceramic composition and method for producing same
CN114835489A (en) * 2022-05-11 2022-08-02 国网智能电网研究院有限公司 Potassium-sodium niobate-based leadless piezoelectric ceramic and preparation method thereof
CN114835489B (en) * 2022-05-11 2023-04-28 国网智能电网研究院有限公司 Potassium sodium niobate-based leadless piezoelectric ceramic and preparation method thereof

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Application publication date: 20161207