CN116813336A - Method for optimizing PZT-based piezoelectric ceramic solid-phase sintering process - Google Patents
Method for optimizing PZT-based piezoelectric ceramic solid-phase sintering process Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 72
- 238000005245 sintering Methods 0.000 title claims abstract description 72
- 239000000919 ceramic Substances 0.000 title claims abstract description 59
- 230000008569 process Effects 0.000 title claims abstract description 48
- 239000007790 solid phase Substances 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 42
- 238000010304 firing Methods 0.000 claims description 5
- 210000001161 mammalian embryo Anatomy 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 125000006850 spacer group Chemical group 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims 1
- 238000005457 optimization Methods 0.000 abstract description 9
- 229910000464 lead oxide Inorganic materials 0.000 abstract description 5
- 239000012071 phase Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 abstract 1
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000000748 compression moulding Methods 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009768 microwave sintering Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
Abstract
The application provides an optimization method of a PZT-based piezoelectric ceramic solid-phase sintering process, which mainly improves a traditional sintering device into a high-lead partial pressure atmosphere device with a double-layer crucible nest in a high-temperature solid-phase sintering stage of piezoelectric ceramic. The guarantee of high lead partial pressure atmosphere reduces the generation of a second phase in the sintering process caused by the volatilization of a large amount of lead, and further relieves the problems of uneven components, low density and the like caused by the volatilization of lead in the ceramic sintering process. The arrangement of the two layers of crucibles can ensure that the high lead atmosphere in the high-temperature sintering process can not be influenced by the high-temperature deformation of the crucible, and is beneficial to environmental protection. Further, lead oxide powder is spread on the edge of the inner crucible, so that the content of lead is fully ensured. In addition, on the basis of stacking a PZT ceramic blank and presintered powder by a traditional solid-phase sintering method, PZT gaskets of an upper layer and a lower layer are added, and the temperature difference in the sintering process is optimized, so that the high-temperature sintering is more uniform and stable. Through the optimization of the PZT-based piezoelectric ceramic solid-phase sintering process in the steps, the experimental setting in the sintering process is adjusted, so that the performance reduction caused by the massive volatilization of lead in the PZT-based piezoelectric ceramic sintering process can be relieved, the optimization mode is concise, the cost is low, and the practicability is strong.
Description
Technical Field
The application relates to the technical field of ceramic sintering, in particular to an optimization method of a PZT-based piezoelectric ceramic solid-phase sintering process.
Background
The piezoelectric ceramic is an important functional material capable of realizing the mutual conversion of electric energy and mechanical energy, has low cost and good adjustability, and is widely applied to various fields of daily life. In the preparation process of the piezoelectric ceramic, powder preparation, compression molding and high-temperature sintering are three important processes. The high-temperature sintering is a key link for preparing ceramics, and the design choice of the sintering process directly influences the mechanical properties such as grain size, density, porosity and the like of the ceramics, and the dielectric and piezoelectric properties.
The piezoelectric ceramic sintering process mainly comprises a plurality of methods such as normal pressure solid phase sintering, hot pressing sintering, hot isostatic pressing sintering, microwave sintering, spark plasma sintering and the like. The normal pressure solid phase sintering is the most widely applied technology in the preparation of PZT-based piezoelectric ceramics due to the characteristics of low cost and good stability. In the conventional solid-phase sintering process design, the sintering temperature of PZT-based piezoelectric ceramics is usually set to about 1100-1300 ℃, and the main components in the ceramic raw materials, pb oxide PbO and Pb 3 O 4 Can volatilize in a large amount at a lower temperature of 900-1000 ℃, so that the problems of component segregation and the like of a final sample are caused, and even a second phase is formed, so that the movement of a crystal boundary and a domain wall is limited, and the related mechanical and piezoelectric properties of the ceramic are seriously affected.
In the traditional solid-phase sintering method of PZT-based piezoelectric ceramics, a certain amount of lead oxide raw material is usually added in the powder preparation stage to avoid massive volatilization of lead at high temperature, but the addition of excessive lead oxide cannot effectively inhibit volatilization of lead. Excessive lead oxide liquid phase can also inhibit grain boundary movement and material diffusion, so that the problem of density reduction of ceramic products occurs. The method has the advantages that the traditional solid-phase sintering method is optimally designed, a new process for improving the performance and the manufacturing stability of the PZT-based piezoelectric ceramic is sought, lead volatilization in the sintering process is reduced, the uniformity of ceramic components is improved, and the method has important significance for mass production and performance stability improvement of the PZT-based piezoelectric ceramic.
Disclosure of Invention
The application aims to provide an optimization method of a PZT-based piezoelectric ceramic solid-phase sintering process, which solves the problem that the performance of ceramic products is easily affected due to the fact that a large amount of lead volatilizes in the PZT-based piezoelectric ceramic solid-phase sintering process.
In order to achieve the above purpose, the application provides an optimization method of a PZT-based piezoelectric ceramic solid phase sintering process, which specifically comprises the following steps:
step one, adding excessive Pb when preparing PZT-based piezoelectric ceramic pre-sintering powder before high-temperature sintering 3 O 4 The powder is used to increase the densification rate during sintering.
Specifically, excess Pb 3 O 4 The proportion of the powder is 1-3%.
Specifically, excess Pb 3 O 4 The proportion of the powder was 1%.
And secondly, placing the PZT blank body in a crucible with a smaller model in a mode of stacking the PZT blank body up and down, and separating the PZT blank body by presintered powder with corresponding components.
Specifically, the PZT ceramic plates with corresponding components are used for replacing pre-sintered powder on the uppermost and the lowermost plates, so that the temperature difference of the intermediate green body in the sintering process is reduced.
Specifically, the stacking number of PZT embryo bodies is 3-5.
In particular, the uppermost and lowermost ceramic sheets are reusable.
Step three, spreading a proper amount of Pb around the blank inside the smaller-sized crucible used in the step two 3 O 4 Powder to provide sufficient lead element compensation during sintering.
And step three, nesting a larger-type crucible with opposite placement directions outside the smaller-type small crucible used in the step two.
Specifically, the larger size crucible in step three should be able to completely cover the crucible used in step two.
Compared with the prior art, the application has the beneficial effects that:
according to the optimization method of the PZT-based piezoelectric ceramic solid-phase sintering process, disclosed by the application, a sintering atmosphere with high lead partial pressure is formed, so that a great deal of volatilization of lead in the traditional solid-phase sintering process is inhibited, the process method is easy to realize, the practicability is high, and the properties of uniformity, compactness and the like of components of ceramic products in the traditional solid-phase sintering process can be effectively improved.
In the solid phase sintering process, a proper amount of Pb in the presintered powder 3 O 4 The powder can form liquid phase in the early and middle stages of sintering to increase the densification rate of PZT-based piezoelectric ceramics. Diffusion coefficients of main elements Pb, zr and Ti in PZT-based piezoelectric ceramics are different, and PbTiO 3 Will preferentially generate PbZrO 3 Can be synthesized at higher temperature, and lead volatilization can lead to PbZrO 3 The synthesis of (3) is not satisfactory to expect, zr precipitation is formed, grain boundary migration and substance diffusion are blocked, and the density of the ceramic is reduced. Inside and outside crucible and Pb with proper allowance 3 O 4 Under the combined action of the powder, a high-temperature sintering atmosphere with high lead partial pressure is formed, the volatilization of excessive lead in the sintering process is inhibited, and meanwhile, the environment is protected. The volatilization of lead is relieved, so that PbZrO during the synthesis process of the PZT-based piezoelectric ceramic 3 The synthesis of the ceramic is smoother, the second phase precipitation at the grain boundary is avoided, and the density and the component uniformity of the ceramic are improved.
The process optimization process only adds a crucible nested structure with lower cost and a small amount of pre-sintered powder to spread, so that the cost of the process optimization is not obviously improved and the process difficulty is lower while the expected ceramic performance requirement is met.
A double-layer nested structure is designed in the sintering process of the PZT-based piezoelectric ceramic to form a high-lead partial pressure sintering atmosphere, so that excessive volatilization of lead is reduced, and the generation of a second phase in the sintering process is avoided to influence the mechanical and piezoelectric properties of the ceramic. The setting of the high lead partial pressure sintering atmosphere is simple, the preparation cost is low, and the effect is obvious.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope of the present application.
FIG. 1 is a schematic diagram of a modified PZT-based piezoceramic solid phase sintering process in accordance with an embodiment of the present application.
Fig. 2 is a detailed view of experimental details of a solid phase sintering process of an improved PZT-based piezoelectric ceramic according to an embodiment of the present application.
Reference numerals:
10-crucible; 20-presintering powder; 30-Pb 3 O 4 A powder; a 40-PZT pad; 50-PZT embryo body.
Detailed Description
Embodiments of the present application are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used in the description of the templates herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
The application provides a method for optimizing a PZT-based piezoelectric ceramic solid phase sintering process, referring to FIG. 1, comprising the following steps: crucible 10, prefiring powder 20, pb 3 O 4 Powder 30, PZT pad 40, PZT green body 50.
Specifically, the crucible 10 is selected as a common high-temperature sintering crucible with different sizes, and the inner and outer crucibles ensure high lead partial pressure in the high-temperature sintering process, and meanwhile, lead is not volatilized in a large amount in the environment to cause environmental pollution.
More specifically, two kinds of crucibles with different sizes are placed in opposite directions, namely the opening and closing directions of the inner crucible are upward, other parts in the solid-phase sintering process are filled, the opening and closing directions of the outer crucible are downward, the smaller inner crucible is nested, and the sintering atmosphere is ensured. The nesting of the inner crucible and the outer crucible ensures the high lead partial pressure atmosphere at high temperature, and avoids the failure of the high lead partial pressure atmosphere caused by the deformation of the inner crucible at high temperature.
The presintered powder 20 and PZT green bodies 50 are alternately stacked in an inner crucible, the PZT shims 40 are placed at the uppermost and lowermost layers, and a proper amount of Pb is spread on the inner edge of the inner crucible 3 O 4 The powder ensures high lead atmosphere and reduces a great deal of volatilization of lead.
Preferably, the presintered powder 20 and the PZT green body are alternately stacked in 3-5 layers, and the proper number of stacked layers can lower the temperature difference during sintering of the green body, so that the influence on the ceramic performance is avoided.
Preferably, the PZT pads 40 are placed on the uppermost and lowermost layers, also with the pre-firing powder as a spacer, spaced from the PZT green body 50.
Preferably, the PZT shim 40 is a ceramic plate of the same composition as the PZT blank 50 to reduce temperature differentials during sintering of the PZT blank 40.
Preferably, pb is added in the balance of 1% 3 O 4 The powder further ensures certain lead element compensation in the sintering process. The proper excessive lead oxide can form liquid phase in the early and middle stages of high-temperature sintering, which is beneficial to improving the density of the ceramic.
Embodiments of the present application will be described in detail below with reference to specific examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present application and should not be construed as limiting the scope of the present application. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
FIG. 1 is a schematic diagram of a method for optimizing a PZT-based piezoceramic solid phase sintering process according to an embodiment of the present application, and as shown in FIG. 1, the solid phase sintering optimizing process mainly includes a crucible 10 and pre-sintered powder 20, wherein the raw materials and experimental facilities are used; 30-Pb 3 O 4 A powder;a 40-PZT pad; 50-PZT embryo body. A size crucible of a proper size is selected, a small crucible is placed with an opening upwards, a PZT green body 50 and presintered powder 20 are stacked in the small crucible, the number of stacked layers is 3-5, and the shapes of the PZT green body 50 and the presintered powder 20 are selected to be common compression molding cylinders. On both the upper and lower sides of the laminate, PZT shims 40 corresponding to the composition of the PZT embryo body 50 are placed, also separated by the pre-firing powder 20. Adding 1% of Pb into the presintered powder 3 O 4 Raw materials are used as element supplements of lead. A layer of Pb is paved at the edge of the bottom of the inner side of the small crucible 3 O 4 The powder 30 is further supplemented with an element of lead. Closing the crucible sealing cover.
After the inner crucible is prevented from being completed, the opening direction of the large crucible of the outer layer is placed downward, so that the two layers of crucibles are nested. Under the condition that the outer crucible can fully contain the inner crucible, the inner crucible is provided with four small crucibles which are placed inside, and sintering efficiency is improved.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and are not limiting; although the application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the application.
Claims (8)
1. The PZT-based piezoelectric ceramic solid phase sintering process optimizing method is characterized by comprising the following steps of:
the double-layer crucible is divided into an inner layer crucible and an outer layer crucible, the bottom is sealed, the upper part is provided with a sealing cover, and the size of the double-layer crucible is enough for the outer layer crucible to be nested into the inner layer crucible;
Pb 3 O 4 powder of Pb 3 O 4 The powder is paved at the bottom edge of the inner crucible.
And the PZT blank body refers to a sintering raw material after the powder configuration of the PZT-based piezoelectric ceramic is completed and pressed.
Presintered powder which is a PZT-based piezoelectric ceramic component ingredient to be processed and added with a part of Pb in balance 3 O 4 The components are as follows.
And the PZT gasket refers to a piezoelectric ceramic sheet which is sintered with the PZT-based piezoelectric ceramic to be processed and has the same component.
2. The method for optimizing the solid phase sintering process of PZT-based piezoelectric ceramics according to claim 1, wherein the double-layered crucible is placed with the opening of the inner crucible facing upward, the opening of the outer crucible facing downward, and the outer crucible can completely cover the inner crucible.
3. The method for optimizing PZT-based piezoelectric ceramic solid phase sintering process according to claim 2, wherein Pb 3 O 4 The powder is paved at the inner edge of the inner crucible and does not contact with the PZT blank, the PZT gasket and the presintered powder.
4. The method for optimizing a solid phase sintering process of a PZT-based piezoelectric ceramic according to claim 3, wherein the PZT green body, the PZT spacer and the pre-sintered powder are stacked alternately in an inner crucible.
5. The method of optimizing a solid phase sintering process of PZT-based piezoelectric ceramics according to claim 4, wherein the PZT green body and the pre-firing powder are stacked with each other by three to five layers.
6. The method of optimizing a PZT-based piezoelectric ceramic solid phase sintering process according to claim 5, wherein the PZT spacer and the pre-firing powder are placed only on the uppermost layer and the lowermost layer of the PZT green body and the pre-firing powder stacked.
7. The method of optimizing a PZT-based piezoelectric ceramic solid phase sintering process according to claim 6, wherein the PZT pad and the PZT embryo body have the same composition, and the PZT pad is reusable.
8. The method for optimizing a solid phase sintering process of PZT-based piezoelectric ceramics according to claim 7, wherein the pre-sintered powder is added with 1% of Pb as a balance 3 O 4 The components are as follows.
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