CN113880574A - PZT-5 type ceramic wafer stacking and sintering method - Google Patents
PZT-5 type ceramic wafer stacking and sintering method Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 105
- 238000005245 sintering Methods 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 30
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 26
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 19
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000010287 polarization Effects 0.000 claims abstract description 13
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000465 moulding Methods 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000007670 refining Methods 0.000 claims abstract description 6
- 235000012431 wafers Nutrition 0.000 claims description 30
- 239000002002 slurry Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 12
- 230000005684 electric field Effects 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 4
- 230000007480 spreading Effects 0.000 claims description 4
- 238000003892 spreading Methods 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 230000002159 abnormal effect Effects 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 230000008878 coupling Effects 0.000 claims description 3
- 238000010168 coupling process Methods 0.000 claims description 3
- 238000005859 coupling reaction Methods 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000000875 high-speed ball milling Methods 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 6
- 238000012545 processing Methods 0.000 description 4
- 239000012814 acoustic material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006355 external stress Effects 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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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
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- 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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Abstract
The invention relates to a PZT-5 type ceramic wafer-based stacking and sintering method, which comprises the following steps: preparing materials; mixing materials; pre-burning; refining powder; plasticizing; molding and plastic removal; preparing a sintering pad, and mixing and grinding the particles of the ceramic green body and zirconium dioxide powder; sintering the ceramic; upper electrode and polarization treatment; and (4) measuring the piezoelectric performance. The invention introduces zirconium dioxide powder on the basis of PZT-5 type piezoelectric ceramic process. The novel sintering padding is prepared by ball milling and mixing the planetary ball mill and PZT-5 type piezoelectric ceramic clinker powder, and is spread on the surface of a green wafer to help to reduce the volatilization of PbO in the wafer, improve the electrical property of the ceramic and improve the phenomenon of wafer adhesion.
Description
Technical Field
The invention relates to a ceramic substrate process technology, in particular to a stack sintering method based on PZT-5 type ceramic wafers,
background
The piezoelectric ceramic material is an extremely important electronic information functional device material, has been developed rapidly in recent years and has become one of indispensable modern industrial materials in the modern time due to the increasingly wide application. The piezoelectric effect is that when external stress is applied to the piezoelectric ceramic material, electric charges (positive piezoelectric property) are generated on the surface of the internal crystal of the piezoelectric ceramic material; if an external electric field is applied to the material, the internal crystal will deform (reverse piezoelectricity) under the action of the electric field. PbO in the piezoelectric ceramic raw material has higher saturated vapor pressure and can volatilize in a gas form at higher sintering temperature. If the Pb loss is too large, the performance of the piezoelectric ceramic material is drastically reduced.
At present, PZT series piezoelectric ceramics as ceramics widely applied to industry are sintered by embedding powder by clinker powder of the same kind of ceramics, although volatilization of PbO in a ceramic wafer can be reduced, the sintered ceramic wafer can generate adhesion phenomenon, and the subsequent processing difficulty is increased. How to reduce the volatilization of PbO during the sintering process and reduce the adhesion phenomenon of the sintered crystal plate has been the research focus of researchers in recent years.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the problems that the sintered ceramic wafer in the prior art can generate adhesion, the subsequent processing difficulty is increased and PbO in the ceramic wafer volatilizes, thereby providing a PZT-5 type ceramic wafer-based stacking sintering method which is slightly influenced by sea conditions and can ensure the overall stability of the wind turbine generator to the greatest extent,
in order to solve the technical problem, the invention discloses a PZT-5 type ceramic wafer-based stacking and sintering method, which comprises the following steps:
step S1: preparing materials: calculating the proportion of each component according to the chemical formula of the ceramic formula;
step S2: mixing materials: ball-milling and mixing materials by adopting a traditional wet method, and adding ceramic powder and deionized water into a stirring barrel according to the mass ratio of 100: 47;
step S3: pre-burning: the process of forming piezoelectric ceramics is a typical chemical reaction process, and at a temperature lower than the melting point, Pb atoms can be diffused into crystals of other materials to form PbZrTiO3；
Step S4: refining powder: weighing the ceramic powder after the pre-sintering treatment, pouring the ceramic powder into deionized water, and uniformly stirring to prepare mixed ceramic slurry;
step S5: plasticizing: taking the thinned ceramic slurry out of the charging barrel; ball-milling and stirring the ceramic slurry and PVA solution which accounts for about 6 percent of the weight of the material, uniformly mixing, then introducing the ceramic slurry into a spray granulator, and sieving the prepared powder by using a 120-mesh screen;
step S6: molding and plastic removal: pre-pressing and molding the powder, and plastic discharging: putting the ceramic green body into a muffle furnace, setting the maximum temperature to be 750 ℃, and further removing a forming agent in the ceramic green body;
step S7: preparing a sintering padding: placing PZT-5 type ceramic green body powder obtained by spray granulation in a crucible and covering the crucible with a cover plate, calcining at 1300 ℃ for 60min, taking out after cooling, putting the mixture into a high-efficiency crusher to be crushed into particles, and mixing and grinding the particles with zirconium dioxide powder;
step S8: and (3) sintering of ceramics: uniformly spreading a sintering padding on the ceramic wafer green body by using a 40-mesh screen, placing the next ceramic green body after uniformly covering, and circulating the operation; setting the sintering temperature to 1310-;
step S9: upper electrode and polarization process, upper electrode: carrying out silver impregnation treatment on the surface of the piezoelectric ceramic to form a metal film, and carrying out polarization treatment: applying a strong direct current electric field to the piezoelectric ceramic;
step S10: and (3) piezoelectric performance measurement: e.g. d33Dielectric loss tan delta and electromechanical coupling coefficient Kp。
In an embodiment of the present invention, in the material mixing step, slurry needs to be stirred in a stirring barrel for 7min in advance, after the low-speed ball milling is performed for 45s, high-speed ball milling is started without abnormal conditions, the ball milling time is set to 3h, and after the ball milling is finished, the slurry is dried for standby.
In one embodiment of the invention, the powder material refining step is to fill the mixed ceramic slurry into a cylinder of a high-efficiency ball mill for secondary refining treatment for 24 hours.
In one embodiment of the invention, the molding and plastic-discharging steps set the wafer to a pre-press molding size of 20x1 mm.
In an embodiment of the invention, in the step of preparing the sintering pad, the calcined particles of the ceramic green body and the zirconium dioxide powder are ball-milled in a planetary ball mill for 2 hours according to a mass ratio of 1:1, the frequency is set to be 200Hz, and the ball-milling medium is 10mm zirconium oxide balls.
In an embodiment of the present invention, after the piezoelectric ceramic is subjected to the polarization treatment step, ferroelectric domains inside the material of the piezoelectric ceramic are turned, all the ferroelectric domains in the piezoelectric ceramic are arranged in the direction of an electric field, and only the piezoelectric ceramic subjected to the polarization treatment has a piezoelectric effect.
Compared with the prior art, the technical scheme of the invention has the following advantages: the invention relates to a PZT-5 type ceramic wafer-based stacking and sintering method, which introduces zirconium dioxide powder on the basis of a PZT-5 type piezoelectric ceramic process. The novel sintering padding is prepared by ball milling and mixing the planetary ball mill and PZT-5 type piezoelectric ceramic clinker powder, and is spread on the surface of a green wafer to help to reduce the volatilization of PbO in the wafer, improve the electrical property of the ceramic and improve the phenomenon of wafer adhesion.
Drawings
In order that the manner in which the present invention is made will be more readily understood, a more particular description of the invention, briefly summarized above, may be had by reference to the embodiments thereof which are illustrated in the appended drawings,
FIG. 1 is a flow chart of a sintering method based on PZT-5 type ceramic wafer stacking.
Detailed Description
As shown in fig. 1, the present embodiment provides a PZT-5 based ceramic wafer stack sintering method, comprising the steps of:
step S1: preparing materials: calculating the proportion of each component according to the chemical formula of the ceramic formula;
step S2: mixing materials: ball-milling and mixing materials by adopting a traditional wet method, and adding ceramic powder and deionized water into a stirring barrel according to the mass ratio of 100: 47;
step S3: pre-burning: generatingThe process of piezoelectric ceramics is a typical chemical reaction process, and Pb atoms can be diffused into crystals of other materials to generate PbZrTiO at a temperature lower than the melting point3；
Step S4: refining powder: weighing the ceramic powder after the pre-sintering treatment, pouring the ceramic powder into deionized water, and uniformly stirring to prepare mixed ceramic slurry;
step S5: plasticizing: taking the thinned ceramic slurry out of the charging barrel; ball-milling and stirring the ceramic slurry and PVA solution which accounts for about 6 percent of the weight of the material, uniformly mixing, then introducing the ceramic slurry into a spray granulator, and sieving the prepared powder by using a 120-mesh screen;
step S6: molding and plastic removal: pre-pressing and molding the powder, and plastic discharging: placing the ceramic green body into a muffle furnace, setting the maximum temperature to be 750 ℃, further removing a forming agent in the ceramic green body, ensuring the sintering quality and improving the sintering density;
step S7: preparing a sintering padding: placing PZT-5 type ceramic green body powder obtained by spray granulation in a crucible and covering the crucible with a cover plate, calcining at 1300 ℃ for 60min, taking out after cooling, putting the mixture into a high-efficiency crusher to be crushed into particles, and mixing and grinding the particles with zirconium dioxide powder;
step S8: and (3) sintering of ceramics: uniformly spreading a sintering padding on the ceramic wafer green body by using a 40-mesh screen, placing the next ceramic green body after uniformly covering, and circulating the operation; setting the sintering temperature as 1340 ℃, preserving the heat for 2 hours, and cooling along with the furnace;
step S9: upper electrode and polarization process, upper electrode: carrying out silver impregnation treatment on the surface of the piezoelectric ceramic to form a metal film, and carrying out polarization treatment: applying a strong direct current electric field to the piezoelectric ceramic;
step S10: and (3) piezoelectric performance measurement: e.g. d33Dielectric loss tan delta and electromechanical coupling coefficient Kp。
Wherein the experimental measurement results of the 20x1mm round wafer are as follows:
the performance parameters of the underwater acoustic material P-5 are as follows:
and (4) conclusion:
because the ceramic clinker powder and the zirconium dioxide powder are used as sintering padding, the phenomena of PbO volatilization and ceramic wafer adhesion of a ceramic green body in the sintering process are reduced during stacking and sintering. The working time of grinding the end face in the subsequent processing is reduced, and the yield is improved. The prepared PZT-5 ceramic material is d at normal temperature33A value of 580pC/N, k at room temperaturep67 percent, has higher performance parameters, and reaches the application standard of the underwater acoustic material.
And in the material mixing step, slurry is required to be stirred in a stirring barrel for 7min in advance, high-speed ball milling is started without abnormal operation after low-speed ball milling is carried out for 45s, the ball milling time is set to be 3h, and the slurry is dried for later use after the ball milling is finished.
In the step of powder material refinement, the mixed ceramic slurry is filled into a charging barrel of a high-efficiency ball mill for secondary refinement treatment for 24 hours.
In the molding and plastic discharging steps, the wafer is pre-pressed to form the wafer with the size of 20x1 mm.
Further, in the step of preparing the sintering padding, calcined particles of the ceramic green body and zirconium dioxide powder are subjected to ball milling for 2 hours in a planetary ball mill according to the mass ratio of 1:1, the frequency is set to be 200Hz, and the ball milling medium is 10mm zirconium oxide balls.
The method greatly reduces the phenomenon of adhesion after ceramic sintering by spreading the special sintering padding, reduces the working time of grinding the end face of the subsequent processing and improves the yield. And simultaneously, the phenomenon that the zirconium dioxide powder absorbs Pb atoms in a green body during sintering is reduced to the maximum extent. The prepared PZT-5 ceramic material has good performance at normal temperature.
After the piezoelectric ceramic is subjected to the polarization treatment step, ferroelectric domains in the piezoelectric ceramic are turned, all the ferroelectric domains in the piezoelectric ceramic are arranged in the direction of an electric field, and only the piezoelectric ceramic subjected to the polarization treatment has the piezoelectric effect.
It is obvious that the above-mentioned embodiments are given by way of example only, and are not limitative of the embodiments, and that, on the basis of the above description, many other variants and modifications are possible to those skilled in the art, which variants and modifications do not require exhaustive enumeration of all embodiments and are therefore obvious and are within the scope of the invention.
Claims (6)
1. A PZT-5 type ceramic wafer based stacking and sintering method is characterized by comprising the following steps:
step S1: preparing materials: calculating the proportion of each component according to the chemical formula of the ceramic formula;
step S2: mixing materials: ball-milling and mixing materials by adopting a traditional wet method, and adding ceramic powder and deionized water into a stirring barrel according to the mass ratio of 100: 47;
step S3: pre-burning: the process of forming piezoelectric ceramics is a typical chemical reaction process, and at a temperature lower than the melting point, Pb atoms can be diffused into crystals of other materials to form PbZrTiO3；
Step S4: refining powder: weighing the ceramic powder after the pre-sintering treatment, pouring the ceramic powder into deionized water, and uniformly stirring to prepare mixed ceramic slurry;
step S5: plasticizing: taking the thinned ceramic slurry out of the charging barrel; ball-milling and stirring the ceramic slurry and PVA solution which accounts for about 6 percent of the weight of the material, uniformly mixing, then introducing the ceramic slurry into a spray granulator, and sieving the prepared powder by using a 120-mesh screen;
step S6: molding and plastic removal: pre-pressing and molding the powder, and plastic discharging: placing the ceramic green body into a muffle furnace, setting the maximum temperature to be 750 ℃, further removing a forming agent in the ceramic green body, ensuring the sintering quality and improving the sintering density;
step S7: preparing a sintering padding: placing PZT-5 type ceramic green body powder obtained by spray granulation in a crucible and covering the crucible with a cover plate, calcining at 1300 ℃ for 60min, taking out after cooling, putting the mixture into a high-efficiency crusher to be crushed into particles, and mixing and grinding the particles with zirconium dioxide powder;
step S8: and (3) sintering of ceramics: uniformly spreading a sintering padding on the ceramic wafer green body by using a 40-mesh screen, placing the next ceramic green body after uniformly covering, and circulating the operation; setting the sintering temperature to 1310-;
step S9: upper electrode and polarization process, upper electrode: carrying out silver impregnation treatment on the surface of the piezoelectric ceramic to form a metal film, and carrying out polarization treatment: applying a strong direct current electric field to the piezoelectric ceramic;
step S10: and (3) piezoelectric performance measurement: e.g. d33Dielectric loss tan delta and electromechanical coupling coefficient Kp。
2. The sintering method for stacking ceramic wafers based on PZT-5 type according to claim 1, wherein: and in the material mixing step, slurry is required to be stirred in a stirring barrel for 7min in advance, high-speed ball milling is started without abnormal operation after low-speed ball milling is carried out for 45s, the ball milling time is set to be 3h, and the slurry is dried for later use after the ball milling is finished.
3. The sintering method for stacking ceramic wafers based on PZT-5 type according to claim 1, wherein: in the step of powder material refinement, the mixed ceramic slurry is filled into a charging barrel of a high-efficiency ball mill for secondary refinement treatment for 24 hours.
4. The sintering method for stacking ceramic wafers based on PZT-5 type according to claim 1, wherein: in the molding and plastic discharging steps, the wafer is pre-pressed to form the wafer with the size of 20x1 mm.
5. The sintering method for stacking ceramic wafers based on PZT-5 type according to claim 1, wherein: in the step of preparing the sintering padding, calcined particles of the ceramic green body and zirconium dioxide powder are subjected to ball milling for 2 hours in a planetary ball mill according to the mass ratio of 1:1, the frequency is set to be 200Hz, and the ball milling medium is 10mm zirconium oxide balls.
6. The sintering method for stacking ceramic wafers based on PZT-5 type according to claim 1, wherein: after the piezoelectric ceramic is subjected to the polarization treatment step, ferroelectric domains in the piezoelectric ceramic are turned, all the ferroelectric domains in the piezoelectric ceramic are arranged in the direction of an electric field, and only the piezoelectric ceramic subjected to the polarization treatment has the piezoelectric effect.
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| CN110862262A (en) * | 2019-12-05 | 2020-03-06 | 湖南嘉业达电子有限公司 | High-performance piezoelectric ceramic applied to sound element and manufacturing method thereof |
| CN112341196A (en) * | 2020-10-27 | 2021-02-09 | 海鹰企业集团有限责任公司 | Novel piezoelectric ceramic powder refining method and piezoelectric ceramic |
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| CN117423549B (en) * | 2023-10-18 | 2024-05-14 | 广东微容电子科技有限公司 | MLCC and MLCC manufacturing method for improving raw inverted adhesive sheet |
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