CN110950658A - Preparation method of power type piezoelectric ceramic capable of being sintered at low temperature - Google Patents
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Abstract
The invention discloses a preparation method of power type piezoelectric ceramics capable of being sintered at low temperature, which comprises the following steps: weighing the ingredients; ball-milling, drying, molding and presintering, wherein a substance R is introduced into the mixed material in the step (3) for presintering; sintering, mixing K2CO3 into the piezoelectric ceramic product sintered in the step (4) for sintering; preserving heat, and cooling the raw materials sintered in the step (5) along with a furnace; and (4) quality detection, namely detecting the piezoelectric ceramic product cooled and formed in the step (6). The preparation method of the power type piezoelectric ceramic capable of being sintered at the low temperature can finish the composition and the process of the sintered power type piezoelectric ceramic material at about 1000 ℃, greatly reduces the energy consumption in the high-temperature sintering process, saves energy, simultaneously avoids the problem that the process is not well controlled by volatilization of substances at the high temperature, improves the efficiency of the control work of workers, facilitates the operation of the workers, has good market prospect and is convenient to popularize and use.
Description
Technical Field
The invention relates to a preparation method of piezoelectric ceramics, in particular to a preparation method of power type piezoelectric ceramics capable of being sintered at low temperature, belonging to the technical field of piezoelectric material application.
Background
Piezoelectric ceramics are information functional ceramic materials capable of mutually converting mechanical energy and electric energy, namely, piezoelectric effect, and have dielectricity, elasticity and the like in addition to piezoelectricity, and are widely applied to medical imaging, acoustic sensors, acoustic transducers, ultrasonic motors and the like.
The power type piezoelectric ceramic belongs to typical hard materials, generally, the required sintering temperature is higher, the sintered ceramic product can be ensured to have better mechanical and electrical properties only when the high temperature reaches about 1260 to 1320, on one hand, the energy consumption is higher in the high-temperature sintering process, on the other hand, the material volatilization is larger at the high temperature, and the process is not easy to control. Therefore, a method for preparing power type piezoelectric ceramics capable of being sintered at low temperature is provided for solving the problems.
Disclosure of Invention
The present invention is directed to a method for preparing a power type piezoelectric ceramic capable of being sintered at a low temperature in order to solve the above problems.
The invention realizes the aim through the following technical scheme, and provides a preparation method of power type piezoelectric ceramics capable of being sintered at low temperature, which comprises the following steps:
(1) weighing the materials, namely weighing the piezoceramic material according to a composition equation [ Pb1-xCaxZr0.52Ti0.47Nb0.01O3+ a% MnCO3 b% R +0.01% K2CO3 ]; wherein a and b% are weight percentage; a is a first additional component with the value of 0.30-2.0; b is a second additional component with the value of 0.5-1.2; weighing x with the value of 0.005-0.05;
(2) ball-milling and drying, namely ball-milling the weighed raw materials on a ball mill for 6 to 8 hours, pouring the ball-milled mixed materials into a tray, and drying the mixed materials in a drying oven at a temperature of between 70 and 80 ℃;
(3) molding, namely putting the mixed material obtained in the step (3) into a pressure test die for briquetting;
(4) pre-sintering, namely introducing a substance R into the mixed material in the step (3) for pre-sintering;
(5) sintering, mixing K2CO3 into the piezoelectric ceramic product sintered in the step (4) for sintering;
(6) preserving heat, and cooling the raw materials sintered in the step (5) along with a furnace;
(7) and (4) quality detection, namely detecting the piezoelectric ceramic product cooled and formed in the step (6).
Preferably, the raw materials weighed in the step (1) are sequentially ball-milled, and the ball-milled raw materials are uniformly mixed.
Preferably, the substance R in the step (1) is introduced in the form of ultrafine powder, and in a most preferred embodiment, Bi-B-Zn frit with a uniform structure is adopted as R, and the frit is processed into ultrafine powder with a median particle size of about 0.5um and then introduced as an accessory ingredient.
Preferably, the pre-sintering in the step (4) is stabilized at a temperature of 750 ℃ to 850 ℃ for a time of 5h to 7 h.
Preferably, the sintering temperature in the step (5) is controlled to be 950 ℃ to 1050 ℃.
Preferably, in the step (3), K2CO3 is introduced, the mass of K2CO3 is weighed, K2CO3 is mixed into the dried mixed material, and the doping amount of K2CO3 is strictly controlled.
The invention has the beneficial effects that: this kind of but low temperature sintering's power type piezoceramics preparation method, can accomplish the power type piezoceramics material composition and the technology of sintering about 1000 degrees, very big reduction in high temperature sintering in-process energy consumption, the energy can be saved, avoid the problem of the good control technology of material volatilization under the high temperature simultaneously, improve the efficiency of worker control work, make things convenient for the worker to operate, simultaneously through introducing K2CO3, and the strict control doping volume, improve the splendid cooling range of ceramic material, the compactness of piezoceramics article has been guaranteed again, good market prospect has, convenient to popularize and use.
Drawings
FIG. 1 is a flow chart of the preparation method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a preparation method of power type piezoelectric ceramics capable of being sintered at low temperature comprises the following steps:
(1) weighing the materials, namely weighing the piezoceramic material according to a composition equation [ Pb1-xCaxZr0.52Ti0.47Nb0.01O3+ a% MnCO3 b% R +0.01% K2CO3 ]; wherein a and b% are weight percentage; a is a first additional component with the value of 0.30-2.0; b is a second additional component with the value of 0.5-1.2; weighing x with the value of 0.005-0.05;
(2) ball-milling and drying, namely ball-milling the weighed raw materials on a ball mill for 6 to 8 hours, pouring the ball-milled mixed materials into a tray, and drying the mixed materials in a drying oven at 75 to 80 ℃;
(3) molding, namely putting the mixed material obtained in the step (3) into a pressure test die for briquetting;
(4) pre-sintering, namely introducing a substance R into the mixed material in the step (3) for pre-sintering;
(5) sintering, mixing K2CO3 into the piezoelectric ceramic product sintered in the step (4) for sintering;
(6) preserving heat, and cooling the raw materials sintered in the step (5) along with a furnace;
(7) and (4) quality detection, namely detecting the piezoelectric ceramic product cooled and formed in the step (6).
Preferably, the raw materials weighed in the step (1) are sequentially ball-milled, and the ball-milled raw materials are uniformly mixed.
Preferably, the substance R in the step (1) is introduced in the form of ultrafine powder, and in a most preferred embodiment, Bi-B-Zn frit with a uniform structure is adopted as R, and the frit is processed into ultrafine powder with a median particle size of about 0.5um and then introduced as an accessory ingredient.
Preferably, the pre-sintering in the step (4) is stabilized at a temperature of 750 ℃ to 800 ℃ for a time of 5h to 7 h.
Preferably, the sintering temperature in the step (5) is controlled to be 950 ℃ to 1000 ℃.
Preferably, in the step (3), K2CO3 is introduced, the mass of K2CO3 is weighed, K2CO3 is mixed into the dried mixed material, and the doping amount of K2CO3 is strictly controlled.
The preparation method of the power type piezoelectric ceramic capable of being sintered at low temperature is suitable for manufacturing piezoelectric ceramic products in large batch.
Example two:
a preparation method of power type piezoelectric ceramics capable of being sintered at low temperature comprises the following steps:
(1) weighing the materials, namely weighing the piezoceramic material according to a composition equation [ Pb1-xCaxZr0.52Ti0.47Nb0.01O3+ a% MnCO3 b% R +0.01% K2CO3 ]; wherein a and b% are weight percentage; a is a first additional component with the value of 0.30-2.0; b is a second additional component with the value of 0.5-1.2; weighing x with the value of 0.005-0.05;
(2) ball-milling and drying, namely ball-milling the weighed raw materials on a ball mill for 6 to 8 hours, pouring the ball-milled mixed materials into a tray, and drying the mixed materials in a drying oven at 75 to 80 ℃;
(3) molding, namely putting the mixed material obtained in the step (3) into a pressure test die for briquetting;
(4) pre-sintering, namely introducing a substance R into the mixed material in the step (3) for pre-sintering;
(5) sintering, mixing K2CO3 into the piezoelectric ceramic product sintered in the step (4) for sintering;
(6) preserving heat, and cooling the raw materials sintered in the step (5) along with a furnace;
(7) and (4) quality detection, namely detecting the piezoelectric ceramic product cooled and formed in the step (6).
Preferably, the raw materials weighed in the step (1) are sequentially ball-milled, and the ball-milled raw materials are uniformly mixed.
Preferably, the substance R in the step (1) is introduced in the form of ultrafine powder, and in a most preferred embodiment, Bi-B-Zn frit with a uniform structure is adopted as R, and the frit is processed into ultrafine powder with a median particle size of about 0.5um and then introduced as an accessory ingredient.
Preferably, the pre-sintering in the step (4) is stabilized at a temperature of 800 ℃ to 850 ℃ for a time of 5h to 7 h.
Preferably, the sintering temperature in the step (5) is controlled to be 950 ℃ to 1050 ℃.
Preferably, in the step (3), K2CO3 is introduced, the mass of K2CO3 is weighed, K2CO3 is mixed into the dried mixed material, and the doping amount of K2CO3 is strictly controlled.
The preparation method of the power type piezoelectric ceramic capable of being sintered at low temperature is suitable for manufacturing small batches of piezoelectric ceramic, and greatly improves the production quality of the piezoelectric ceramic.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. A preparation method of power type piezoelectric ceramics capable of being sintered at low temperature is characterized by comprising the following steps: the preparation method of the power type piezoelectric ceramic capable of being sintered at low temperature comprises the following steps:
(1) weighing the materials, namely weighing the piezoceramic material according to a composition equation [ Pb1-xCaxZr0.52Ti0.47Nb0.01O3+ a% MnCO3 b% R +0.01% K2CO3 ]; wherein a and b% are weight percentage; a is a first additional component with the value of 0.30-2.0; b is a second additional component with the value of 0.5-1.2; weighing x with the value of 0.005-0.05;
(2) ball-milling and drying, namely ball-milling the weighed raw materials on a ball mill for 6 to 8 hours, pouring the ball-milled mixed materials into a tray, and drying the mixed materials in a drying oven at a temperature of between 70 and 80 ℃;
(3) molding, namely putting the mixed material obtained in the step (3) into a pressure test die for briquetting;
(4) pre-sintering, namely introducing a substance R into the mixed material in the step (3) for pre-sintering;
(5) sintering, mixing K2CO3 into the piezoelectric ceramic product sintered in the step (4) for sintering;
(6) preserving heat, and cooling the raw materials sintered in the step (5) along with a furnace;
(7) and (4) quality detection, namely detecting the piezoelectric ceramic product cooled and formed in the step (6).
2. The method for preparing power type piezoelectric ceramics capable of being sintered at low temperature according to claim 1, wherein the method comprises the following steps: and (2) ball-milling the weighed raw materials in the step (1) in sequence, and uniformly mixing the ball-milled raw materials.
3. The method for preparing power type piezoelectric ceramics capable of being sintered at low temperature according to claim 1, wherein the method comprises the following steps: in the step (1), the substance R is introduced in an ultrafine powder mode, and in the most preferred embodiment, the substance R adopts Bi-B-Zn frit with a uniform structure, the frit is processed into ultrafine powder with the median particle size of about 0.5um, and then the ultrafine powder is introduced as an accessory ingredient.
4. The method for preparing power type piezoelectric ceramics capable of being sintered at low temperature according to claim 1, wherein the method comprises the following steps: the pre-sintering in the step (4) is stabilized at the temperature of 750 ℃ to 850 ℃ for 5h to 7 h.
5. The method for preparing power type piezoelectric ceramics capable of being sintered at low temperature according to claim 1, wherein the method comprises the following steps: the sintering temperature in the step (5) is controlled to be 950 ℃ to 1050 ℃.
6. The method for preparing power type piezoelectric ceramics capable of being sintered at low temperature according to claim 1, wherein the method comprises the following steps: introducing K2CO3 in the step (3), weighing the mass of K2CO3, mixing K2CO3 into the dried mixed material, and strictly controlling the doping amount of K2CO 3.
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| CN1661827A (en) * | 2004-01-27 | 2005-08-31 | 松下电器产业株式会社 | Piezoelectic element and method for manufacturing the same, and ink jet head and ink jet recording apparatus using the piezoelectric element |
| CN101820569A (en) * | 2010-03-19 | 2010-09-01 | 张家港市玉同电子科技有限公司 | Formula of multilayer piezoelectric ceramic for loudspeaker drive and production method thereof |
| CN102113144A (en) * | 2008-07-31 | 2011-06-29 | 富士胶片株式会社 | Piezoelectric device, piezoelectric device manufacturing method, and liquid discharge apparatus |
| CN102299253A (en) * | 2010-06-25 | 2011-12-28 | 富士胶片株式会社 | Piezoelectric film, piezoelectric device and liquid ejection apparatus |
| CN103693966A (en) * | 2013-12-13 | 2014-04-02 | 云南云天化股份有限公司 | Low temperature co-fired ceramic material and preparation method thereof |
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- 2018-09-27 CN CN201811132229.5A patent/CN110950658A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1661827A (en) * | 2004-01-27 | 2005-08-31 | 松下电器产业株式会社 | Piezoelectic element and method for manufacturing the same, and ink jet head and ink jet recording apparatus using the piezoelectric element |
| CN102113144A (en) * | 2008-07-31 | 2011-06-29 | 富士胶片株式会社 | Piezoelectric device, piezoelectric device manufacturing method, and liquid discharge apparatus |
| CN101820569A (en) * | 2010-03-19 | 2010-09-01 | 张家港市玉同电子科技有限公司 | Formula of multilayer piezoelectric ceramic for loudspeaker drive and production method thereof |
| CN102299253A (en) * | 2010-06-25 | 2011-12-28 | 富士胶片株式会社 | Piezoelectric film, piezoelectric device and liquid ejection apparatus |
| CN103693966A (en) * | 2013-12-13 | 2014-04-02 | 云南云天化股份有限公司 | Low temperature co-fired ceramic material and preparation method thereof |
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