CN113501710A - Preparation method of sodium bismuth titanate textured ceramic - Google Patents
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Abstract
The invention provides a preparation method of sodium bismuth titanate textured ceramic, which comprises the following steps: s1: synthesizing ceramic matrix powder by a solid phase method; s2: synthesizing flaky template crystal grains by a two-step molten salt method; s3: mixing the base powder obtained in the step S1 with the template grains obtained in the step S2; s4: granulating the mixed powder obtained in the step S3, and filling the granulated particles into a die and pressing into a ceramic green body; s5: and (5) carrying out glue discharging and sintering on the ceramic green body obtained in the step S4 to obtain the textured ceramic. The method has the advantages of simple process, easy operation and low cost, saves the experiment cost and the equipment investment, and can prepare the textured ceramic with higher texture degree and excellent piezoelectric performance.
Description
Technical Field
The invention belongs to the technical field of preparation of sodium bismuth titanate, and particularly relates to a preparation method of sodium bismuth titanate textured ceramic.
Background
Piezoelectric materials are functional materials for realizing mutual conversion between electric energy and mechanical energy, and functional converters such as sensors, brakes, accelerators, actuators and the like manufactured by the piezoelectric materials play an important role in the fields of heat, force, sound, light, electricity, magnetism, humidity and the like. Compared with common piezoelectric ceramics, the piezoelectric single crystal has extremely high anisotropy, so the piezoelectric effect of the piezoelectric single crystal is far better than that of the piezoelectric ceramics. However, the preparation process of the piezoelectric single crystal is complex, the cost is high, the period is long, and the preparation of the large-size single crystal is difficult, which seriously restricts the wide application of the piezoelectric single crystal. Researchers hope to realize a piezoelectric ceramic which is simple and feasible in the aspect of preparation process and is comparable to piezoelectric single crystal in the aspect of piezoelectric performance, so that the excellent performance of the piezoelectric single crystal is combined with the simple preparation process of the piezoelectric ceramic, and a novel piezoelectric ceramic, namely a textured ceramic, is obtained.
The existing preparation method of the textured ceramic mainly comprises a heat treatment technology; magnetic field orientation techniques; a template grain growth technique; and (3) a reaction template growth technology. The preparation processes have more flows and complex experimental processes.
Disclosure of Invention
The invention provides a preparation method of sodium bismuth titanate textured ceramic, aiming at solving the problems of more flows and complex experimental process of the existing preparation method of textured ceramic.
The invention adopts the following technical scheme:
a preparation method of sodium bismuth titanate textured ceramic comprises the following steps:
s1: synthesizing ceramic matrix powder by a solid phase method;
s2: synthesizing flaky template crystal grains by a two-step molten salt method;
s3: mixing the base powder obtained in the step S1 with the template grains obtained in the step S2;
s4: granulating the mixed powder obtained in the step S3, and putting the granulated particles into a die for dry pressing and forming to obtain a ceramic green body;
s5: and (5) carrying out glue discharging and sintering on the ceramic green body obtained in the step S4 to obtain the textured ceramic.
Further, when the solid phase method is used for the synthesis in step S1, the method includes the steps of:
s11: with Na2CO3、Bi2O3And TiO2As raw material according to Bi1/2Na1/2TiO3Weighing and preparing powder according to the stoichiometric ratio of the chemical formula;
s12: ball-milling the powder for 4 hours by taking absolute ethyl alcohol as a medium;
s13: and drying the ball-milled powder, and sintering the powder at 800 ℃ for 2 h.
Further, the step of synthesizing the plate-shaped template crystal grains by using the two-step molten salt method in the step S2 includes the following steps:
s21: with Bi2O3And TiO2As raw material according to Bi4Ti3O12Weighing and proportioning the materials according to the stoichiometric ratio of the chemical formula to obtain powder;
s22: ball-milling the powder for 4 hours by using absolute ethyl alcohol as a medium, and adding sodium chloride with the total mass ratio of 1:1 to the powder during ball-milling;
s23: drying the ball-milled powder, sintering for 2h at the temperature of 960 ℃, and then cleaning the obtained product to obtain Bi4Ti3O12A precursor;
s24: with Bi4Ti3O12Precursor, Na2CO3And TiO2As raw material according to Bi1/2Na1/2TiO3Weighing the prepared materials according to the stoichiometric ratio of the chemical formula;
s25: ball-milling the prepared materials for 4 hours by using absolute ethyl alcohol as a medium, and adding sodium chloride with the total mass ratio of the materials being 1:1 during ball-milling;
s26: drying the ball-milled materials, sintering at 900 ℃ for 2h, and cleaning the obtained product to obtain Bi1/2Na1/2TiO3Template grains.
Further, in step S3, the mass ratio of the matrix powder to the template crystal grains is 1:1 when mixing is performed.
Further, in step S4, a uniaxial pressing device is used for pressing by dry pressing, and a 6mm × 6mm steel mold is used as the mold.
Further, the pressure is 10 Mpa-30 Mpa during dry pressing, and the pressure is maintained for 1 min-10 min.
Further, in step S5, a double-layered alumina crucible is used and sintering is performed by the method of homogenous powder burial.
Further, in step S5, the conditions for discharging the glue are: keeping the temperature at 600 ℃ for 4 h.
Further, in step S5, the sintering conditions are: heating to 960 ℃ at the rate of 3 ℃ per min, preserving heat for 2h, and naturally cooling along with the furnace.
The invention has the beneficial effects that: the invention provides a novel method for preparing textured ceramic, namely a dry pressing method, based on a hot pressing technology. The method has the advantages of simple process, easy operation and low cost, saves the experiment cost and the equipment investment, and can prepare the textured ceramic with higher texture degree and excellent piezoelectric performance.
Drawings
FIG. 1 is an SEM image of a sodium bismuth titanate textured ceramic prepared in example 1;
FIG. 2 is an SEM image of a sodium bismuth titanate textured ceramic prepared in example 2;
FIG. 3 is an SEM image of the sodium bismuth titanate textured ceramic prepared in example 3.
Detailed Description
The present invention is further described with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the claims, and other alternatives which may occur to those skilled in the art are also within the scope of the claims.
Example 1:
this example is Bi1/2Na1/2TiO3As a matrix, with a flake Bi1/2Na1/2TiO3The specific preparation method of the template crystal grain comprises the following steps:
s1: mixing Na2CO3、Bi2O3And TiO2The raw material is according to Bi1/2Na1/2TiO3Weighing the ingredients in a chemical formula to prepare powder, and ball-milling the powder for 4 hours by taking absolute ethyl alcohol as a medium. And drying the ball-milled powder, putting the dried powder into an alumina crucible, and sintering the powder at the temperature of 800 ℃ for 2 h. Preparation of Bi1/2Na1/2TiO3A matrix powder.
S2: adding Bi2O3And TiO2Powder is according to Bi4Ti3O12Chemical formula is adopted for proportioning and weighing to obtain powder (due to Bi)2O3Is easy to volatilize, so Bi is used for weighing the material2O3Excessive 10 wt%), adding sodium chloride with the mass ratio of 1:1 to the powder, and ball-milling the powder for 4 hours by taking absolute ethyl alcohol as a medium. And drying the ball-milled powder, putting the dried powder into an alumina crucible, sintering the powder at the temperature of 960 ℃ for 2h, and repeatedly washing the obtained product with deionized water. Preparation of Bi4Ti3O12And (3) precursor.
Weighing a certain amount of Bi according to the molar ratio of 1:2:54Ti3O12Precursor, Na2CO3And TiO2Preparing materials from the powder, adding sodium chloride in a mass ratio of 1:1 to the total powder, and ball-milling the prepared materials for 4 hours by using absolute ethyl alcohol as a medium. Drying the ball-milled materials, putting the dried ball-milled materials into an alumina crucible, sintering the ball-milled materials at 900 ℃ for 2h, and cleaning an unnecessary reaction product Bi by hydrochloric acid2O3Then repeatedly washing with deionized water for several times to prepare the flaky Bi1/2Na1/2TiO3Template grains.
S3: weighing Bi according to the mass ratio of 1:11/2Na1/2TiO3Matrix powder and Bi1/2Na1/2TiO3And (5) carrying out ball milling on the template grains and uniformly mixing.
S4: and then granulating to obtain granules with larger granularity and good fluidity. And (3) loading the granulated particles into a 6mm multiplied by 6mm steel mould by adopting a uniaxial pressure device, applying 10MPa pressure, and maintaining the pressure for 1min to prepare the ceramic green body with the parallel arrangement of the template crystal grains.
S5: the obtained ceramic green body is subjected to heat preservation at 600 ℃ for 4h for glue discharging, then is sintered at 960 ℃, is naturally cooled along with a furnace, and texture Bi is prepared1/2Na1/2TiO3A ceramic.
Texture Bi in example 11/2Na1/2TiO3The ceramics achieve the following performance indexes: sintering the mixture into porcelain at 960 ℃, wherein the texture degree is 60 percent.
Example 2:
this example is Bi1/2Na1/2TiO3As a matrix, with a flake Bi1/2Na1/2TiO3The specific preparation method of the template crystal grain comprises the following steps:
s1: mixing Na2CO3、Bi2O3And TiO2The raw material is according to Bi1/2Na1/2TiO3Weighing the ingredients in a chemical formula to prepare powder, and ball-milling the powder for 4 hours by taking absolute ethyl alcohol as a medium. And drying the ball-milled powder, putting the dried powder into an alumina crucible, and sintering the powder at the temperature of 800 ℃ for 2 h. Preparation of Bi1/2Na1/2TiO3A matrix powder.
S2: adding Bi2O3And TiO2Powder is according to Bi4Ti3O12Chemical formula is adopted for proportioning and weighing to obtain powder (due to Bi)2O3Is easy to volatilize, so Bi is used for weighing the material2O3Excessive 10 wt%), adding sodium chloride with the mass ratio of 1:1 to the powder, and ball-milling the powder for 4 hours by taking absolute ethyl alcohol as a medium. And drying the ball-milled powder, putting the dried powder into an alumina crucible, sintering the powder at the temperature of 960 ℃ for 2h, and repeatedly washing the obtained product with deionized water. Preparation of Bi4Ti3O12And (3) precursor.
Weighing a certain amount of Bi according to the molar ratio of 1:2:54Ti3O12Precursor, Na2CO3And TiO2Preparing materials from the powder, adding sodium chloride in a mass ratio of 1:1 to the total powder, and ball-milling the prepared materials for 4 hours by using absolute ethyl alcohol as a medium. Drying the ball-milled materials, putting the dried ball-milled materials into an alumina crucible, sintering the ball-milled materials at 900 ℃ for 2h, and cleaning an unnecessary reaction product Bi by hydrochloric acid2O3Then repeatedly washing with deionized water for several times to prepare the flaky Bi1/2Na1/2TiO3Template grains.
S3: weighing Bi according to the mass ratio of 1:11/2Na1/2TiO3Matrix powder and Bi1/2Na1/2TiO3Template particles and ball milling are carried outMixing uniformly.
S4: and then granulating to obtain granules with larger granularity and good fluidity. And (3) loading the granulated particles into a 6mm multiplied by 6mm steel mould by adopting a uniaxial pressure device, applying 20MPa pressure, and maintaining the pressure for 5min to prepare the ceramic green body with the parallel arrangement of the template crystal grains.
S5: the obtained ceramic green body is subjected to heat preservation at 600 ℃ for 4h for glue discharging, then is sintered at 960 ℃, is naturally cooled along with a furnace, and texture Bi is prepared1/2Na1/2TiO3A ceramic.
Texture Bi in example 20.4Na0.6TiO3The ceramics achieve the following performance indexes: sintering the mixture into porcelain at 960 ℃, wherein the texture degree is 70%.
Example 3:
this example is Bi1/2Na1/2TiO3As a matrix, with a flake Bi1/2Na1/2TiO3Is a template, and the specific preparation method comprises the following steps:
s1: mixing Na2CO3、Bi2O3And TiO2The raw material is according to Bi1/2Na1/2TiO3Weighing the ingredients in a chemical formula to prepare powder, and ball-milling the powder for 4 hours by taking absolute ethyl alcohol as a medium. And drying the ball-milled powder, putting the dried powder into an alumina crucible, and sintering the powder at the temperature of 800 ℃ for 2 h. Preparation of Bi1/2Na1/2TiO3A matrix powder.
S2: adding Bi2O3And TiO2Powder is according to Bi4Ti3O12Chemical formula is adopted for proportioning and weighing to obtain powder (due to Bi)2O3Is easy to volatilize, so Bi is used for weighing the material2O3Excessive 10 wt%), adding sodium chloride with the mass ratio of 1:1 to the powder, and ball-milling the powder for 4 hours by taking absolute ethyl alcohol as a medium. And drying the ball-milled powder, putting the dried powder into an alumina crucible, sintering the powder at the temperature of 960 ℃ for 2h, and repeatedly washing the obtained product with deionized water. Preparation of Bi4Ti3O12And (3) precursor.
Weighing a certain amount of Bi according to the molar ratio of 1:2:54Ti3O12Precursor, Na2CO3And TiO2Preparing materials from the powder, adding sodium chloride in a mass ratio of 1:1 to the total powder, and ball-milling the prepared materials for 4 hours by using absolute ethyl alcohol as a medium. Drying the ball-milled materials, putting the dried ball-milled materials into an alumina crucible, sintering the ball-milled materials at 900 ℃ for 2h, and cleaning an unnecessary reaction product Bi by hydrochloric acid2O3Then repeatedly washing with deionized water for several times to prepare the flaky Bi1/2Na1/2TiO3Template grains.
S3: weighing Bi according to the mass ratio of 1:11/2Na1/2TiO3Base and Bi1/2Na1/2TiO3And (5) performing ball milling on the template and uniformly mixing.
S4: and then granulating to obtain granules with larger granularity and good fluidity. And (3) loading the granulated particles into a 6mm multiplied by 6mm steel mould by adopting a uniaxial pressure device, applying 30MPa pressure, and maintaining the pressure for 10min to prepare the ceramic green body with the parallel arrangement of the template crystal grains.
S5: the obtained ceramic green body is subjected to heat preservation at 600 ℃ for 4h for glue discharging, then is sintered at 960 ℃, is naturally cooled along with a furnace, and texture Bi is prepared1/2Na1/2TiO3A ceramic.
Texture Bi in example 31/2Na1/2TiO3The ceramics achieve the following performance indexes: sintering the mixture into porcelain at 960 ℃, wherein the texture degree is 74%.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (9)
1. The preparation method of the sodium bismuth titanate textured ceramic is characterized by comprising the following steps:
s1: synthesizing ceramic matrix powder by a solid phase method;
s2: synthesizing flaky template crystal grains by a two-step molten salt method;
s3: mixing the base powder obtained in the step S1 with the template grains obtained in the step S2;
s4: granulating the mixed powder obtained in the step S3, and putting the granulated particles into a die for dry pressing and forming to obtain a ceramic green body;
s5: and (5) carrying out glue discharging and sintering on the ceramic green body obtained in the step S4 to obtain the textured ceramic.
2. The method for preparing the sodium bismuth titanate textured ceramic of claim 1, which is characterized in that: when the solid phase method is used for synthesis in step S1, the method includes the steps of:
s11: with Na2CO3、Bi2O3And TiO2As raw material according to Bi1/2Na1/2TiO3Weighing and preparing powder according to the stoichiometric ratio of the chemical formula;
s12: ball-milling the powder for 4 hours by taking absolute ethyl alcohol as a medium;
s13: and drying the ball-milled powder, and sintering the powder at 800 ℃ for 2 h.
3. The method for preparing the sodium bismuth titanate textured ceramic of claim 1, which is characterized in that: the step S2 of synthesizing the flaky template crystal grain by using a two-step molten salt method comprises the following steps:
s21: with Bi2O3And TiO2As raw material according to Bi4Ti3O12Weighing and proportioning the materials according to the stoichiometric ratio of the chemical formula to obtain powder;
s22: ball-milling the powder for 4 hours by using absolute ethyl alcohol as a medium, and adding sodium chloride with the total mass ratio of 1:1 to the powder during ball-milling;
s23: drying the ball-milled powder, sintering for 2h at the temperature of 960 ℃, and then cleaning the obtained product to obtain Bi4Ti3O12A precursor;
s24: with Bi4Ti3O12Precursor, Na2CO3And TiO2As raw material according to Bi1/2Na1/2TiO3Weighing the prepared materials according to the stoichiometric ratio of the chemical formula;
s25: ball-milling the prepared materials for 4 hours by using absolute ethyl alcohol as a medium, and adding sodium chloride with the total mass ratio of the materials being 1:1 during ball-milling;
s26: drying the ball-milled materials, sintering at 900 ℃ for 2h, and cleaning the obtained product to obtain Bi1/2Na1/2TiO3Template grains.
4. The method for preparing the sodium bismuth titanate textured ceramic of claim 1, which is characterized in that: in step S3, the mass ratio of the matrix powder to the template grains is 1:1 when mixing is performed.
5. The method for preparing the sodium bismuth titanate textured ceramic of claim 1, which is characterized in that: in step S4, a uniaxial pressing machine was used for the dry pressing, and a 6mm × 6mm steel mold was used as the mold.
6. The method for preparing the sodium bismuth titanate textured ceramic of claim 1, which is characterized in that: and (3) keeping the pressure for 1-10 min at 10-30 Mpa during dry pressing.
7. The method for preparing the sodium bismuth titanate textured ceramic of claim 1, which is characterized in that: in step S5, a double-layered alumina crucible is used and sintering is performed by the method of burying homogeneous powder.
8. The method for preparing the sodium bismuth titanate textured ceramic of claim 1, which is characterized in that: in step S5, the conditions for removing the glue are: keeping the temperature at 600 ℃ for 4 h.
9. The method for preparing the sodium bismuth titanate textured ceramic of claim 1, which is characterized in that: in step S5, the sintering conditions are: heating to 960 ℃ at the rate of 3 ℃ per min, preserving heat for 2h, and naturally cooling along with the furnace.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115072773A (en) * | 2022-06-16 | 2022-09-20 | 西安交通大学 | Template for textured lead zirconate titanate-based ceramic and preparation method thereof |
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| CN1850725A (en) * | 2006-05-23 | 2006-10-25 | 青岛大学 | Method for preparing polycrystal texture ceramic material |
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| CN115072773A (en) * | 2022-06-16 | 2022-09-20 | 西安交通大学 | Template for textured lead zirconate titanate-based ceramic and preparation method thereof |
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Application publication date: 20211015 |