CN112234138A - Preparation method of large-size multilayer piezoelectric ceramic - Google Patents

Preparation method of large-size multilayer piezoelectric ceramic Download PDF

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Publication number
CN112234138A
CN112234138A CN202011168250.8A CN202011168250A CN112234138A CN 112234138 A CN112234138 A CN 112234138A CN 202011168250 A CN202011168250 A CN 202011168250A CN 112234138 A CN112234138 A CN 112234138A
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ceramic
screen printing
temperature
multilayer piezoelectric
piezoelectric ceramic
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CN202011168250.8A
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CN112234138B (en
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赵兵
段连威
彭大松
李文文
宫丹丹
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Chinese Sensor Technology (qingdao) Academy Of Science
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Chinese Sensor Technology (qingdao) Academy Of Science
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    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10NELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00Piezoelectric or electrostrictive devices
    • H10N30/80Constructional details
    • H10N30/85Piezoelectric or electrostrictive active materials
    • H10N30/853Ceramic compositions
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • HELECTRICITY
    • H10SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10NELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00Piezoelectric or electrostrictive devices
    • H10N30/01Manufacture or treatment
    • H10N30/05Manufacture of multilayered piezoelectric or electrostrictive devices, or parts thereof, e.g. by stacking piezoelectric bodies and electrodes
    • H10N30/057Manufacture of multilayered piezoelectric or electrostrictive devices, or parts thereof, e.g. by stacking piezoelectric bodies and electrodes by stacking bulk piezoelectric or electrostrictive bodies and electrodes

Abstract

The invention discloses a preparation method of large-size multilayer piezoelectric ceramics, which comprises the process steps of punching a casting diaphragm, silk-screen printing, laminating, isostatic pressing, cutting, glue discharging, sintering, polarizing and the like. The invention relates to the field of multilayer piezoelectric ceramic manufacturing. The preparation method provided by the invention is suitable for preparing the multilayer piezoelectric ceramic piece with the length of more than 3cm and the width of more than 3cm, and the application of the piezoelectric ceramic piece in the field of large drive is expanded.

Description

Preparation method of large-size multilayer piezoelectric ceramic
Technical Field
The invention relates to the field of preparation of piezoelectric ceramic pieces, in particular to a preparation process of multilayer piezoelectric ceramic.
Background
The piezoelectric ceramic has the advantages of high control precision, high response speed, good linearity, low power consumption and the like, and is widely applied to the fields of electronics, communication, medicine and the like. With the development of science, when the single-layer piezoelectric ceramic is used, the voltage is high, the displacement is small, the requirement of high thrust under the current low voltage cannot be met, and in order to overcome the defects, the multilayer piezoelectric ceramic attracts more and more attention.
At present, the length of the common multilayer piezoelectric ceramic product is less than 3cm, the width of the common multilayer piezoelectric ceramic product is less than 3cm, and the common multilayer piezoelectric ceramic product does not meet the use requirement under the condition of some large displacement requirements. And the bigger laminated piezoelectric ceramic piece has the defect that in the glue discharging process, internal organic matters are not easy to discharge, so that the sample piece is damaged due to bubbles.
Technical problem to be solved
The invention provides a preparation method of large-size multilayer piezoelectric ceramics, which is realized by designing the thickness of an electrode, adjusting the binding force between laminated layers and sheets during isostatic pressing and adopting a special glue discharging and sintering process.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method of large-size multilayer piezoelectric ceramics specifically comprises the following steps:
step one, a punching machine is selected to punch a positioning hole on the ceramic wafer;
step two, screen printing is carried out on the ceramic chip with the punched holes, the mesh number of screen printing patterns is 400-500 meshes, the screen printing plate patterns with the wire diameter of 18-22 mu m are printed, the screen printing distance is 1-2mm, the included angle between a scraper and the screen printing plate is 30-60 degrees, the thickness of printing silver paste is 4-6 mu m, and the thickness of the sintered silver paste is 1-2 mu m;
step three, carrying out hot-pressing lamination on the ceramic plate after silk-screen printing, wherein the temperature of an upper pressing plate is 55-60 ℃, the temperature of a lower pressing plate is 45-48 ℃, the laminating time is 30-40s, and the laminating pressure is 3000-;
step four, carrying out warm isostatic pressing on the multilayer ceramic wafer, wherein the water temperature is 55-65 ℃, the pressure is increased for 5min, the pressure is maintained for 10-15min, and the pressure is 4500-5500 psi;
step five, cutting the multi-layer ceramic wafer subjected to isostatic pressing according to a designed cutting line, and putting the cut ceramic wafer into a glue discharging furnace for a glue discharging experiment, wherein the glue discharging curve is as follows: the heating rate is 1 ℃/min, the temperature is raised to 200 ℃ and kept for 4h, then the heating rate is adjusted to 0.5 ℃/min, the temperature is raised to 450-;
step seven, putting the multilayer ceramic chip after the glue is discharged into a sintering furnace for sintering, wherein the sintering curve is as follows: heating to 500 ℃ at a heating rate of 1 ℃/min, keeping the temperature for 3h, adjusting the heating rate to 0.5 ℃/min, heating to 925 ℃ and 950 ℃, keeping the temperature for 3h, and cooling along with the furnace;
and step eight, polarizing the sintered multilayer piezoelectric ceramics by selecting an air polarization mode.
Preferably, in the cutting process, the cutting line is 2mm long and 0.2mm wide.
Preferably, in the glue discharging process, in order to ensure the air permeability of the bottom surface of the ceramic wafer, piezoelectric ceramic powder with the thickness of 3mm is paved at the lower part of the ceramic wafer.
(III) advantageous effects
The invention provides a preparation method of large-size multilayer piezoelectric ceramic, and a piezoelectric ceramic piece with the length of more than 3cm and the width of more than 3cm is prepared, so that the application of the piezoelectric ceramic in large-displacement driving is expanded.
Drawings
FIG. 1 is a schematic structural view of a multilayer piezoelectric ceramic according to the present invention;
FIG. 2 is a cross-sectional view of a laminated 30-layer ceramic sheet of 5 x 4cm prepared by the present invention;
in FIG. 1, 1 is an internal electrode, 2 is a single-layer ceramic sheet, 3 is a surface electrode, 4 is 5cm in length direction, and 5 is 4cm in width.
Detailed Description
The described embodiments are only some, not all embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The embodiment of the invention provides a technical scheme that: a preparation method for large-size multilayer piezoelectric ceramics specifically comprises the following steps:
step one, a punching machine is selected to punch a positioning hole on the ceramic wafer;
step two, screen printing is carried out on the ceramic wafer with the punched holes, the mesh number of screen printing patterns is 500 meshes, screen printing plate patterns with the line diameter of 18 microns are printed, the screen printing distance is 2mm, the included angle between a scraper and the screen printing plate is 45 degrees, the thickness of printing silver paste is 5 microns, and the thickness of the sintered silver paste is 1.5 microns;
step three, carrying out hot-pressing lamination on the ceramic wafer subjected to silk-screen printing, wherein the temperature of an upper pressing plate is 55 ℃, the temperature of a lower pressing plate is 45 ℃, the laminating time is 30s, and the laminating pressure is 3500 psi;
step four, carrying out warm isostatic pressing on the multilayer ceramic wafer, wherein the water temperature is 60 ℃, the pressure is increased for 5min, the pressure is maintained for 10min, and the pressure is 5000 psi;
step five, cutting the multi-layer ceramic wafer subjected to isostatic pressing according to a designed cutting line;
sixthly, putting the cut ceramic wafer into a glue discharging furnace for glue discharging experiments, wherein the glue discharging curve is as follows: the heating rate is 1 ℃/min, the temperature is raised to 200 ℃, the temperature is kept for 4h, then the heating rate is adjusted to 0.5 ℃/min, the temperature is raised to 450 ℃, the temperature is kept for 8h, and the furnace cooling is carried out;
step seven, putting the multilayer ceramic chip after the glue is discharged into a sintering furnace for sintering, wherein the sintering curve is as follows: heating to 500 deg.C at a heating rate of 1 deg.C/min, maintaining for 3 hr, adjusting the heating rate to 0.5 deg.C/min, heating to 30 deg.C, maintaining for 3 hr, and cooling with the furnace.
And step eight, polarizing the sintered multilayer piezoelectric ceramics by selecting an air polarization mode.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (3)

1. A preparation method of large-size multilayer piezoelectric ceramics is characterized in that a sintering process with reasonable inner electrode thickness, proper lamination temperature isostatic pressing process and lower binder removal temperature and slower heating rate is selected, and comprises the following steps:
step one, a punching machine is selected to punch a positioning hole on the ceramic wafer;
step two, screen printing is carried out on the ceramic chip with the punched holes, the mesh number of screen printing patterns is 400-500 meshes, the screen printing plate patterns with the wire diameter of 18-22 mu m are printed, the screen printing distance is 1-2mm, the included angle between a scraper and the screen printing plate is 30-60 degrees, the thickness of printing silver paste is 4-6 mu m, and the thickness of the sintered silver paste is 1-2 mu m;
step three, carrying out hot-pressing lamination on the ceramic plate after silk-screen printing, wherein the temperature of an upper pressing plate is 55-60 ℃, the temperature of a lower pressing plate is 45-48 ℃, the laminating time is 30-40s, and the laminating pressure is 3000-;
step four, carrying out warm isostatic pressing on the multilayer ceramic wafer, wherein the water temperature is 55-65 ℃, the pressure is increased for 5min, the pressure is maintained for 10-15min, and the pressure is 4500-5500 psi;
step five, cutting the multi-layer ceramic wafer subjected to isostatic pressing according to a designed cutting line;
sixthly, putting the cut ceramic wafer into a glue discharging furnace for glue discharging experiments, wherein the glue discharging curve is as follows: the heating rate is 1 ℃/min, the temperature is raised to 200 ℃ and kept for 4h, then the heating rate is adjusted to 0.5 ℃/min, the temperature is raised to 450-;
step seven, putting the multilayer ceramic chip after the glue is discharged into a sintering furnace for sintering, wherein the sintering curve is as follows: heating to 500 deg.C at a rate of 1 deg.C/min, maintaining for 3h, adjusting the heating rate to 0.5 deg.C/min, heating to 925 deg.C and 950 deg.C, maintaining for 3h, and cooling with furnace
And step eight, polarizing the sintered multilayer piezoelectric ceramics by selecting an air polarization mode.
2. A method for producing a large-sized multilayer piezoelectric ceramic according to claim 1, characterized in that: in the cutting process, the length of the cutting line is 2mm, and the width of the cutting line is 0.2 mm.
3. A method for producing a large-sized multilayer piezoelectric ceramic according to claim 1, characterized in that: in the glue discharging process, in order to ensure the air permeability of the bottom surface of the ceramic chip during glue discharging, piezoelectric ceramic powder with the thickness of 3mm is paved on the lower part of the ceramic chip.
CN202011168250.8A 2020-10-28 2020-10-28 Preparation method of large-size multilayer piezoelectric ceramic Active CN112234138B (en)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06334236A (en) * 1993-05-20 1994-12-02 Fujitsu Ltd Manufacture of multilayer piezoelectric/electrostrictive actuator
JP2003282994A (en) * 2002-03-27 2003-10-03 Denso Corp Method for manufacturing laminate type piezoelectric element
JP2007103676A (en) * 2005-10-04 2007-04-19 Tdk Corp Piezoelectric ceramic composition, and laminated piezoelectric element and its manufacturing method
CN101456733A (en) * 2008-09-24 2009-06-17 陕西师范大学 Method for preparing potassium niobate sodium base leadless piezoelectric ceramic thin sheet and application thereof in buzzer
CN108275999A (en) * 2018-04-02 2018-07-13 齐鲁工业大学 A kind of preparation method of potassium niobate sodium-based leadless piezoelectric ceramic
CN108358629A (en) * 2018-01-27 2018-08-03 天津大学 The preparation of low temperature co-fired self-supporting PZT bases multi-layer piezoelectric thick film
CN109053196A (en) * 2018-07-12 2018-12-21 中国电子科技集团公司第五十五研究所 A kind of sintering method of large scale high-temperature co-fired ceramics
CN110835266A (en) * 2019-12-03 2020-02-25 池州学院 Potassium-sodium niobate-based piezoelectric ceramic and preparation method and application thereof
CN111533556A (en) * 2020-04-28 2020-08-14 太原理工大学 Preparation method of grain-oriented strontium sodium niobate leadless ferroelectric ceramic
CN111682102A (en) * 2020-05-29 2020-09-18 深圳振华富电子有限公司 Preparation method of piezoelectric driver stack

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06334236A (en) * 1993-05-20 1994-12-02 Fujitsu Ltd Manufacture of multilayer piezoelectric/electrostrictive actuator
JP2003282994A (en) * 2002-03-27 2003-10-03 Denso Corp Method for manufacturing laminate type piezoelectric element
JP2007103676A (en) * 2005-10-04 2007-04-19 Tdk Corp Piezoelectric ceramic composition, and laminated piezoelectric element and its manufacturing method
CN101456733A (en) * 2008-09-24 2009-06-17 陕西师范大学 Method for preparing potassium niobate sodium base leadless piezoelectric ceramic thin sheet and application thereof in buzzer
CN108358629A (en) * 2018-01-27 2018-08-03 天津大学 The preparation of low temperature co-fired self-supporting PZT bases multi-layer piezoelectric thick film
CN108275999A (en) * 2018-04-02 2018-07-13 齐鲁工业大学 A kind of preparation method of potassium niobate sodium-based leadless piezoelectric ceramic
CN109053196A (en) * 2018-07-12 2018-12-21 中国电子科技集团公司第五十五研究所 A kind of sintering method of large scale high-temperature co-fired ceramics
CN110835266A (en) * 2019-12-03 2020-02-25 池州学院 Potassium-sodium niobate-based piezoelectric ceramic and preparation method and application thereof
CN111533556A (en) * 2020-04-28 2020-08-14 太原理工大学 Preparation method of grain-oriented strontium sodium niobate leadless ferroelectric ceramic
CN111682102A (en) * 2020-05-29 2020-09-18 深圳振华富电子有限公司 Preparation method of piezoelectric driver stack

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