CN112194464A - Sintering method for lead-containing piezoelectric ceramic product - Google Patents
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Abstract
The invention discloses a sintering method for a lead-containing piezoelectric ceramic product, and relates to the technical field of sintering of the lead-containing piezoelectric ceramic product. The sintering method for the lead-containing piezoelectric ceramic product is matched with a method of burying sintering and double-crucible cover sintering to complete the sintering process of the lead-containing piezoelectric ceramic product, the piezoelectric ceramic product with good flatness and less lead loss can be obtained by sintering according to the process, and a brand-new burying sintering and double-crucible cover sintering process is adopted to realize simultaneous sintering of a plurality of products at one time, so that the sintering efficiency is improved, and the product performance is ensured. The comparative experiment shows that the lead-containing piezoelectric ceramic chip which is not buried and sintered by using the powder has obvious bending deformation, and the ceramic chip buried and sintered by using the powder has good flatness; the color of the lead-containing piezoelectric ceramic chip sintered by the buried burning and double-crucible cover burning mode is obviously deeper than that of the lead-containing piezoelectric ceramic chip sintered without the outer crucible cover, which indicates that the outer crucible cover burning has a good lead volatilization prevention effect. Experiments prove that the PZT powder for burying and burning can be recycled, and the cost is further reduced.
Description
Technical Field
The invention relates to the technical field of lead-containing piezoelectric ceramics, in particular to a sintering mode for a lead-containing piezoelectric ceramic product.
Background
The piezoelectric ceramic is a polycrystalline body formed by sintering an oxide mixture (zirconia, lead oxide, titanium oxide, etc.) at a high temperature and performing a solid-phase reaction, and is a ferroelectric ceramic having a piezoelectric effect by a direct-current high-voltage polarization treatment. Piezoelectric ceramics, as an important functional material with force, heat, electricity and light sensitivity, has been widely used in the fields of sensors, ultrasonic transducers, micro-displacers, other electronic components and the like. In various lead-containing piezoelectric ceramic materials applied to the current industry, the content of lead oxide accounts for about 60 percent of the total mass of the materials, and the lead oxide is volatile at high temperature, so that the content of lead in the components is changed, and the product performance is influenced.
The existing lead-containing piezoelectric ceramic product is generally sintered in a direct sintering mode, a stacking sintering mode and a burying sintering mode, lead in the ceramic product is volatilized in the three modes in different degrees, the flatness of a sample wafer cannot be guaranteed, and the volatilization of lead can influence components in the product and further influence the performance of the product. The invention innovatively adopts a sintering mode of buried burning and double-crucible cover burning, thereby reducing the lead volatilization to the maximum extent and ensuring the flatness of the product.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a sintering mode for the lead-containing piezoelectric ceramic product, solves the problems of serious lead volatilization and product flatness during high-temperature sintering in direct sintering, stacked sintering and buried sintering modes, and ensures the stable performance of the lead-containing piezoelectric ceramic product after sintering.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: a sintering mode for a lead-containing piezoelectric ceramic product specifically comprises the following steps:
step one, preparing a crucible: placing the crucible on a clean and flat burning bearing plate;
step two, scattering a first layer of PZT powder: scattering a first layer of PZT powder at the bottom of the crucible, and leveling the PZT powder by using a scraper;
placing the first piezoelectric ceramic product to be fired and scattering a second layer of PZT powder: placing the piezoelectric ceramic product to be fired in the middle of PZT powder, scattering a layer of PZT powder on the piezoelectric ceramic sheet to be fired, and scraping the powder by using a scraper to lightly press the powder to ensure that the piezoelectric ceramic product to be fired is buried in the PZT powder and is not exposed;
step four, placing a second piezoelectric ceramic product to be fired and scattering a third layer of PZT powder: repeating the third step;
putting a third piezoelectric ceramic product to be fired and scattering a fourth layer of PZT powder: repeating the third step;
putting a fourth piezoelectric ceramic product to be fired and scattering fifth layer PZT powder: repeating the third step, and scattering PZT powder on the uppermost layer of the piezoelectric ceramic product, wherein the scattering amount is two to three times of that in the previous step;
step seven, covering the crucible cover: covering the crucible cover tightly, wherein no obvious gap is formed on the side surface, and scattering a layer of PZT powder on the outer edge of the crucible;
step eight, reversely buckling a second crucible: reversely buckling a larger crucible outside the first crucible, scattering a layer of PZT powder on the outer edge of the opening of the crucible, and uniformly covering the outer edge of the contact opening of the crucible and the burning bearing plate with the PZT powder without obvious gaps;
step nine, sintering: sintering the lead-containing piezoelectric ceramic product in a sintering furnace according to a curve of a preset sintering temperature.
Preferably, the setter plate needs to be clean and flat, and the inner size of the crucible is larger than that of the piezoelectric ceramic product, so that the ceramic product can be placed in the crucible.
Preferably, the composition of the PZT powder should be consistent with the piezoelectric ceramic article to be sintered.
Preferably, the piezoelectric ceramic product to be fired is placed in the middle of the PZT powder, and the scraping plate is used for scraping and lightly pressing after the powder is scattered, so that the piezoelectric ceramic product to be fired is not exposed when being buried in the PZT powder, and the amount of the PZT powder on the top layer is two to three times of that in the previous step.
Preferably, the sealing performance between the crucible cover and the crucible is good, no obvious gap appears on the side surface after the crucible cover is covered, and a layer of PZT powder is scattered on the outer edge of the crucible to ensure that the interior of the crucible contains lead in the sintering process.
Preferably, the size of the inverted crucible is larger than that of the first crucible, and the outer edge of the contact opening of the inverted crucible and the burning bearing plate is uniformly covered by PZT powder without obvious gaps.
(III) advantageous effects
The invention provides a sintering method for a lead-containing piezoelectric ceramic product. Compared with the prior art, the method has the following beneficial effects:
the sintering mode for the lead-containing piezoelectric ceramic product specifically comprises the following steps:
step one, preparing a crucible: placing the crucible on a clean and flat burning bearing plate;
step two, scattering a first layer of PZT powder: scattering a first layer of PZT powder at the bottom of the crucible, and leveling the PZT powder by using a scraper;
placing the first piezoelectric ceramic product to be fired and scattering a second layer of PZT powder: placing the piezoelectric ceramic product to be fired in the middle of PZT powder, scattering a layer of PZT powder on the piezoelectric ceramic sheet to be fired, and scraping the powder by using a scraper to lightly press the powder to ensure that the piezoelectric ceramic product to be fired is buried in the PZT powder and is not exposed;
step four, placing a second piezoelectric ceramic product to be fired and scattering a third layer of PZT powder: repeating the third step;
putting a third piezoelectric ceramic product to be fired and scattering a fourth layer of PZT powder: repeating the third step;
putting a fourth piezoelectric ceramic product to be fired and scattering fifth layer PZT powder: repeating the third step, and scattering PZT powder on the uppermost layer of the piezoelectric ceramic product, wherein the scattering amount is two to three times of that in the previous step;
step seven, covering the crucible cover: covering the crucible cover tightly, wherein no obvious gap is formed on the side surface, and scattering a layer of PZT powder on the outer edge of the crucible;
step eight, reversely buckling a second crucible: reversely buckling a larger crucible outside the first crucible, scattering a layer of PZT powder on the outer edge of the opening of the crucible, and uniformly covering the outer edge of the contact opening of the crucible and the burning bearing plate with the PZT powder without obvious gaps;
step nine, sintering: sintering the lead-containing piezoelectric ceramic product in a sintering furnace according to a curve of a preset sintering temperature.
The sintering method for the lead-containing piezoelectric ceramic product mainly uses two sets of crucibles, PZT powder and the piezoelectric ceramic product to be sintered, completes the sintering process of the lead-containing piezoelectric ceramic product by matching the modes of burying sintering and double-crucible cover sintering, can obtain the piezoelectric ceramic product with good flatness and less lead loss according to the process sintering, and realizes the simultaneous sintering of a plurality of products at one time by adopting the brand-new burying sintering and double-crucible cover sintering process, thereby improving the sintering efficiency and ensuring the product performance. The comparative experiment shows that the lead-containing piezoelectric ceramic chip which is not buried and sintered by using the powder has obvious bending deformation, and the ceramic chip buried and sintered by using the powder has good flatness; the color of the lead-containing piezoelectric ceramic chip sintered by the buried burning and double-crucible cover burning mode is obviously deeper than that of the lead-containing piezoelectric ceramic chip sintered without the outer crucible cover, which indicates that the outer crucible cover burning has a good lead volatilization prevention effect. Experiments prove that the PZT powder for burying and burning can be recycled, and the cost is further reduced.
Drawings
FIG. 1 is a schematic view of the present invention;
FIG. 2 is a schematic diagram of a first embodiment of the present invention;
FIG. 3 is a schematic structural view of step two of the present invention;
FIG. 4 is a schematic structural view of step three of the present invention;
FIG. 5 is a schematic structural view of step four of the present invention;
FIG. 6 is a schematic structural view of step five of the present invention;
FIG. 7 is a schematic structural view of step six of the present invention;
FIG. 8 is a schematic structural view of step seven of the present invention;
FIG. 9 is a schematic structural view of step eight of the present invention;
FIG. 10 is a photograph of a piezoelectric ceramic sheet containing lead sintered without burying (left) and with burying (right) powder;
FIG. 11 is a photograph of a piezoelectric ceramic plate containing lead which was sintered without using the outermost crucible cover firing (left) and the double crucible cover firing (right).
In the figure, 1 is a firing plate, 2 is a crucible, 3 is PZT powder, 4 is a to-be-fired ceramic product, 5 is PZT powder, 6 is a to-be-fired ceramic product, 7 is PZT powder, 8 is a to-be-fired ceramic product, 9 is PZT powder, 10 is a to-be-fired ceramic product, 11 is PZT powder, 12 is a crucible cover, 13 is a crucible, 14 is PZT powder, and 15 is PZT powder.
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 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.
Referring to fig. 1 to 11, an embodiment of the present invention provides a technical solution: a sintering mode for a lead-containing piezoelectric ceramic product specifically comprises the following steps:
step one, preparing a crucible: placing the crucible on a clean and flat burning bearing plate;
step two, scattering a first layer of PZT powder: scattering a first layer of PZT powder at the bottom of the crucible, and leveling the PZT powder by using a scraper;
placing the first piezoelectric ceramic product to be fired and scattering a second layer of PZT powder: placing the piezoelectric ceramic product to be fired in the middle of PZT powder, scattering a layer of PZT powder on the piezoelectric ceramic sheet to be fired, and scraping the powder by using a scraper to lightly press the powder to ensure that the piezoelectric ceramic product to be fired is buried in the PZT powder and is not exposed;
step four, placing a second piezoelectric ceramic product to be fired and scattering a third layer of PZT powder: repeating the third step;
putting a third piezoelectric ceramic product to be fired and scattering a fourth layer of PZT powder: repeating the third step;
putting a fourth piezoelectric ceramic product to be fired and scattering fifth layer PZT powder: repeating the third step, and scattering PZT powder on the uppermost layer of the piezoelectric ceramic product, wherein the scattering amount is two to three times of that in the previous step;
step seven, covering the crucible cover: covering the crucible cover tightly, wherein no obvious gap is formed on the side surface, and scattering a layer of PZT powder on the outer edge of the crucible;
step eight, reversely buckling a second crucible: reversely buckling a larger crucible outside the first crucible, scattering a layer of PZT powder on the outer edge of the opening of the crucible, and uniformly covering the outer edge of the contact opening of the crucible and the burning bearing plate with the PZT powder without obvious gaps;
step nine, sintering: sintering the lead-containing piezoelectric ceramic product in a sintering furnace according to a curve of a preset sintering temperature.
The sintering method for the lead-containing piezoelectric ceramic product mainly uses two sets of crucibles, PZT powder and the piezoelectric ceramic product to be sintered, completes the sintering process of the lead-containing piezoelectric ceramic product by matching the modes of burying sintering and double-crucible cover sintering, can obtain the piezoelectric ceramic product with good flatness and less lead loss according to the process sintering, and realizes the simultaneous sintering of a plurality of products at one time by adopting the brand-new burying sintering and double-crucible cover sintering process, thereby improving the sintering efficiency and ensuring the product performance. As can be seen from fig. 10, the lead-containing piezoelectric ceramic sheet not subjected to the burying firing with powder on the left side is significantly deformed by bending, while the ceramic sheet subjected to the burying firing with powder on the right side is good in flatness. As can be seen from FIG. 11, the color of the piezoelectric ceramic sheet containing lead sintered by the buried firing and double-crucible cover firing method on the right side is obviously deeper than that of the piezoelectric ceramic sheet containing lead sintered by the non-outside crucible cover on the left side, which indicates that the outside crucible cover firing has a good effect of preventing lead volatilization, and the lead component in the ceramic sheet is volatilized because no outside crucible protects the lead atmosphere during the sintering process of the ceramic sheet on the left side. Experiments prove that the PZT powder for burying and burning can be recycled, and the cost is further reduced.
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 (6)
1. A sintering method for a lead-containing piezoelectric ceramic product is characterized in that: the method specifically comprises the following steps:
step one, preparing a crucible: placing the crucible on a clean and flat burning bearing plate;
step two, scattering a first layer of PZT powder: scattering a first layer of PZT powder at the bottom of the crucible, and leveling the PZT powder by using a scraper;
placing the first piezoelectric ceramic product to be fired and scattering a second layer of PZT powder: placing the piezoelectric ceramic product to be fired in the middle of PZT powder, scattering a layer of PZT powder on the piezoelectric ceramic product to be fired, and scraping the powder by using a scraper to lightly press the powder to ensure that the piezoelectric ceramic product to be fired is buried in the PZT powder and is not exposed;
step four, placing a second piezoelectric ceramic product to be fired and scattering a third layer of PZT powder: repeating the third step;
putting a third piezoelectric ceramic product to be fired and scattering a fourth layer of PZT powder: repeating the third step;
putting a fourth piezoelectric ceramic product to be fired and scattering fifth layer PZT powder: repeating the third step, and scattering PZT powder on the uppermost layer of the piezoelectric ceramic product, wherein the scattering amount is two to three times of that in the previous step;
step seven, covering the crucible cover: covering the crucible cover tightly, wherein no obvious gap is formed on the side surface, and scattering a layer of PZT powder on the outer edge of the crucible;
step eight, reversely buckling a second crucible: reversely buckling a larger crucible outside the first crucible, scattering a layer of PZT powder on the outer edge of the opening of the crucible, and uniformly covering the outer edge of the contact opening of the crucible and the burning bearing plate with the PZT powder without obvious gaps;
step nine, sintering: sintering the lead-containing piezoelectric ceramic product in a sintering furnace according to a curve of a preset sintering temperature.
2. The sintering method according to claim 1, wherein the sintering method comprises: the burning bearing plate needs to be clean and flat, the size of the inside of the crucible needs to be larger than that of the piezoelectric ceramic product, and the ceramic product can be placed in the crucible.
3. The sintering method according to claim 1, wherein the sintering method comprises: the PZT powder composition needs to be consistent with the piezoelectric ceramic article to be sintered.
4. The sintering method according to claim 1, wherein the sintering method comprises: the piezoelectric ceramic product to be fired is placed in the middle of the PZT powder, and light pressure is stricken off by a scraper after the powder is scattered, so that the piezoelectric ceramic product to be fired is not exposed when being buried in the PZT powder, and the amount of the PZT powder on the top layer is two to three times of that in the previous step.
5. The sintering method according to claim 1, wherein the sintering method comprises: the sealing performance between the crucible cover and the crucible is good, no obvious gap is formed on the side surface, a layer of PZT powder is scattered on the outer edge of the crucible, and the lead-containing atmosphere in the crucible is ensured in the sintering process.
6. The sintering method according to claim 1, wherein the sintering method comprises: the size of the inverted crucible is larger than that of the first crucible, and a layer of PZT powder is uniformly sprayed on the outer edge of the opening of the inverted crucible without obvious gaps.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Application publication date: 20210108 |