CN109796205B - Bismuth-layer-structured bismuth titanium tantalate high-temperature piezoelectric ceramic material and preparation method thereof - Google Patents
Bismuth-layer-structured bismuth titanium tantalate high-temperature piezoelectric ceramic material and preparation method thereof Download PDFInfo
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Abstract
The disclosure relates to a bismuth layerA structural titanium bismuth tantalate high-temperature piezoelectric ceramic material and a preparation method thereof belong to the technical field of high-temperature piezoelectric ceramic materials, and the general formula of the high-temperature piezoelectric ceramic material is Bi3‑ xCexTiTaO9Wherein x is more than 0 and less than or equal to 0.20. The preparation method comprises the following steps: with Bi2O3Powder, TiO2Powder, Ta2O5Powder and CeO2The powder is used as a raw material, and is subjected to pre-ball milling, drying, sintering, secondary ball milling, ceramic blank sheet preparation, plastic discharge and sintering to obtain a high-temperature piezoelectric ceramic material, the obtained blank sheet is polished, the upper surface and the lower surface of the blank sheet are coated with silver electrodes by a silver firing treatment method after polishing, and the blank sheet is subjected to polarization treatment after silver firing treatment to obtain Bi with a bismuth layer structure3TiTaO9High temperature piezoelectric ceramics. Having a piezoelectric constant d of 12-16pC/N33。
Description
Technical Field
The invention belongs to the technical field of high-temperature piezoelectric ceramic materials, and particularly relates to a bismuth titanium tantalate high-temperature piezoelectric ceramic material with a bismuth layer structure and a preparation method thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The piezoelectric ceramics as sensor, brake and frequency converter are widely used in the fields of industrial control, environmental monitoring, communication, information system and medical appliance. In the field of piezoelectric ceramics, the piezoelectric material widely used at present is mainly PZT (PbZrO) having a perovskite structure3-PbTiO3) A material.
However, PZT (PbZrO)3-PbTiO3) The material is a lead-containing ceramic in which lead oxide (or lead tetraoxide) accounts for about 70% of the total mass of the raw material. The lead-containing piezoelectric ferroelectric ceramic can bring harm to the environment and human beings in the processing, sintering and using processes. Therefore, the development of lead-free environment-compatible piezoceramic materials is an urgent and scientifically significant issue.
At present, the lead-free piezoelectric ceramic systems studied at home and abroad mainly comprise: barium titanate-based, sodium bismuth titanate-based, alkali metal niobate-based, bismuth layer-structured, tungsten bronze-structured lead-free piezoelectric ceramics. The bismuth-layer-structured lead-free piezoelectric ceramic material, as a ferroelectric material, has the characteristics of photoelectric effect, nonlinear optical effect, anomalous photovoltaic effect, photorefractive effect and the like, and has the advantages of high curie temperature, high polarization strength, good fatigue resistance, small leakage current and the like, so that the bismuth-layer-structured lead-free piezoelectric ceramic material is valued by researchers. However, the piezoelectric properties of the bismuth-layer structured lead-free piezoelectric ceramics are not ideal.
BRIEF SUMMARY OF THE PRESENT DISCLOSURE
In view of the problems in the prior art, it is an object of the present disclosure to provide a bismuth titanium tantalate high-temperature piezoelectric ceramic material with a bismuth layer structure.
In order to solve the above technical problem, the technical scheme of the present disclosure is:
a bismuth titanium tantalate high-temperature piezoelectric ceramic material with a bismuth layer structure, wherein the general formula of the high-temperature piezoelectric ceramic material is Bi3- xCexTiTaO9Wherein x is more than 0 and less than or equal to 0.20.
In the formula, subscript numbers represent the molar ratio of the elements.
In some embodiments, x is 0.02, 0.05, 0.1.
The bismuth titanium tantalate high-temperature piezoelectric ceramic material with the bismuth layer structure has a piezoelectric constant d of 12-16pC/N33. Curie temperature of 870-885 ℃ and QmIs 8200-12500, QmReflecting the mechanical loss capability, Q, of the piezoelectric materialmThe larger the mechanical loss is, the smaller the mechanical loss is, the better the performance of the bismuth titanium tantalate high-temperature piezoelectric ceramic material prepared by the method has better application in all aspects.
The beneficial effect of this disclosure:
the bismuth titanium tantalate high-temperature piezoelectric ceramic material with the bismuth layer structure disclosed by the invention improves the piezoelectric property of the bismuth titanium tantalate high-temperature piezoelectric ceramic material without reducing the Curie temperature of the bismuth titanium tantalate high-temperature piezoelectric ceramic material, and is a novel environment-friendly piezoelectric ceramic material. And the preparation method has simple process and convenient operation, and is suitable for large-scale industrial production.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this disclosure, are included to provide a further understanding of the disclosure, and are incorporated in and constitute a part of this disclosure.
Fig. 1 is an SEM scanning electron microscope picture of the Ce-substituted bismuth titanium tantalate piezoelectric ceramic material prepared in example 2 of the present disclosure.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. 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 disclosure belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The bismuth layer structured ceramic material is composed of (Bi)2O2)2+The layers and the lattice layers of perovskite structure are alternately superposed, and the chemical general formula is (Bi)2O2)2+(Am-1BmO3m+1)2-In the above formula, A is an ion suitable for 12 coordination, such as Na+、K+、Ca2+Etc., B is an ion suitable for 8 coordination, such as Ti4+、Nb5+And m is an integer and takes the value of 1-5. Bismuth titanium tantalate (Bi)3TiTaO9) Is a bismuth layer structure material with m-2, the Curie temperature of which reaches 890 ℃, and the piezoelectric constant d33About 4pC/N, dielectric loss tan delta<2%, compared with the practical application, the Curie temperature meets the requirement of use at high temperature, but the piezoelectric performance of the piezoelectric ceramic material does not meet the application requirement. Therefore, how to obtain a bismuth-layered piezoelectric ceramic material that can be stably used in a high temperature range by increasing the piezoelectric constant without lowering the curie temperature has become an important issue in the art. At present, the methodNo report on improving the performance of the bismuth titanium tantalate high-temperature piezoelectric ceramic material with the bismuth layer structure by replacing Bi with Ce is found, so that the research and development of the high-temperature piezoelectric ceramic material with excellent performance has great practical value.
In the bismuth titanium tantalate high-temperature piezoelectric ceramic material disclosed by the invention, the element Bi is replaced by the element Ce, and the addition amount of the doping element is optimized, so that the piezoelectric property of the bismuth titanium tantalate high-temperature piezoelectric ceramic material is effectively improved. It should be noted that although there are many reports on element doping of piezoelectric ceramic materials in the prior art, different doping elements and different addition amounts of the doping elements have a great influence on the overall performance of the piezoelectric ceramic materials, which needs to be continuously searched in the test process and obtained through repeated tests, and the inventors have tried substitution and doping modification of bismuth titanium tantalate high-temperature piezoelectric ceramic materials by various elements in the previous research, but compared with substitution and doping of other elements, the bismuth titanium tantalate high-temperature piezoelectric ceramic material with the bismuth layer structure prepared by using the Ce element of the present invention to substitute the Bi element shows more excellent piezoelectric performance.
A bismuth titanium tantalate high-temperature piezoelectric ceramic material with a bismuth layer structure, wherein the general formula of the high-temperature piezoelectric ceramic material is Bi3- xCexTiTaO9Wherein x is more than 0 and less than or equal to 0.20.
In the formula, subscript numbers represent the molar ratio of the elements.
In some embodiments, x is 0.02, 0.05, 0.1.
A preparation method of a bismuth titanium tantalate high-temperature piezoelectric ceramic material with a bismuth layer structure comprises the following specific steps:
with Bi2O3Powder, TiO2Powder, Ta2O5Powder and CeO2The powder is taken as a raw material, and is prepared according to the stoichiometric ratio of Bi, Ti, Ta and Ce in the general formula, and is subjected to pre-ball milling to obtain mixed powder;
drying the mixed powder, and then performing presintering to obtain presintering powder;
performing secondary ball milling on the pre-sintered powder to obtain powder subjected to secondary ball milling;
adding a bonding agent into the powder subjected to the secondary ball milling to press the powder into ceramic blank sheets, and performing plastic removal treatment;
and sintering the ceramic blank sheet after the plastic removal treatment, and cooling to obtain the high-temperature piezoelectric ceramic material.
In some embodiments, the ball milling media of the pre-ball milling and the secondary ball milling is deionized water.
The dosage of the deionized water is 80-100% of the total weight of the raw materials. In the invention, deionized water is used as raw material Bi2O3、TiO2、Ta2O5And CeO2The solvent and the addition of the deionized water are optimized, and the raw materials can be fully ball-milled under the dosage of the invention.
In some embodiments, the ball milling rate of the pre-ball milling and the secondary ball milling is 200-.
The ball milling time is 12-24 h. The ball milling speed and the ball milling time can fully ball mill the raw materials to a certain fineness, and are favorable for pressing the subsequent ceramic blank sheets.
In some embodiments, the drying temperature of the mixed powder after the pre-ball milling is 100-; .
The mixed powder is dried at the temperature, and the main purpose is to remove the deionized water added in the pre-ball milling.
In some embodiments, the pre-sintering temperature is 800-.
The presintering temperature and the heat preservation time are optimized, so that the high-temperature piezoelectric ceramic material with the composition of the general formula can be prepared under the condition, and the temperature stability of the piezoelectric property of the high-temperature bismuth titanium tantalate piezoelectric ceramic material can be further improved through presintering.
In some embodiments, the binder is a 5% by weight aqueous solution of polyvinyl alcohol.
In some embodiments, the binder is present in an amount of 6 to 8% by weight based on the total weight of the powder after the second ball milling.
The adhesive with the amount can be used for fully bonding the mixed powder.
In some embodiments, the plastic ejection temperature is 600-700 ℃.
In some embodiments, the sintering temperature is 1000-.
In the invention, the sintering temperature is controlled, which is beneficial to the bismuth titanium tantalate high-temperature piezoelectric ceramic material to form a single-phase structure.
In some embodiments, the sintering ramp rate is 4-6 ℃/min.
In the present disclosure, the temperature rise rate of sintering is effectively controlled, so that the integrity of the ceramic green sheet can be ensured, and if the temperature rise is too fast, the ceramic green sheet can be cracked.
A preparation method of bismuth titanium tantalate high-temperature piezoelectric ceramic with a bismuth layer structure comprises the following specific steps:
polishing the high-temperature piezoelectric ceramic blank sheet, coating silver electrodes on the upper and lower surfaces of the blank sheet by a silver burning treatment method after polishing, and polarizing the blank sheet after silver burning treatment to obtain Bi with a bismuth layer structure3TiTaO9High temperature piezoelectric ceramics.
In some embodiments, the silver firing treatment temperature is 500-600 ℃, and the holding time of the silver firing treatment is 1-2 h.
In some embodiments, the temperature of the polarization treatment is 150-200 ℃, the voltage of polarization is 10-12kV/mm, and the time of polarization is 20-40 min.
Under the polarization treatment condition, the Ce element substituted bismuth layer-structured bismuth titanium tantalate high-temperature piezoelectric ceramic material can be fully polarized, and the piezoelectric property of the material is improved.
The disclosure is further illustrated with reference to the following examples
Example 1:
preparation of Bi of chemical composition2.98Ce0.02TiTaO9And x is 0.02 of Ce substituted modified bismuth titanium tantalate leadless piezoelectric ceramics.
Analytically pure powder raw material Bi2O3、TiO2、Ta2O5And CeO2According to the followingAnd (2) proportioning the raw materials according to a chemical ratio, mixing the weighed raw materials with deionized water, performing ball milling for 12 hours, presintering for 3 hours at 850 ℃, performing secondary ball milling for 12 hours after crushing, pressing into thin wafers with the diameter of 12mm after drying and grinding, performing plastic discharge at 650 ℃, and performing sintering and heat preservation for 3 hours at 1100 ℃ to obtain the Ce-substituted modified bismuth titanium tantalate leadless piezoelectric ceramic. And polishing the surface of the obtained ceramic sample, coating an Ag electrode on the upper surface and the lower surface of the ceramic sample, polarizing for 30min in silicone oil at 200 ℃ under the direct current voltage of 12kV/mm, and testing the piezoelectric property of the ceramic sample. Piezoelectric constant d of the obtained ceramic sample3312pC/N, 98 dielectric constant epsilon, 0.2 dielectric loss tan delta, and electromechanical coupling coefficient kp8.5%, mechanical quality factor Qm＝8200。
Example 2:
preparation of Bi of chemical composition2.95Ce0.05TiTaO9And x is 0.05 of Ce substituted modified bismuth titanium tantalate leadless piezoelectric ceramics.
Analytically pure powder raw material Bi2O3、TiO2、Ta2O5And CeO2The materials are proportioned according to the chemical proportion, weighed raw materials are mixed with deionized water and then are ball-milled for 12 hours, pre-sintered for 3 hours at 850 ℃, crushed and then are ball-milled for 12 hours for the second time, the crushed materials are pressed into thin wafers with the diameter of 12mm after being dried and ground, and the wafers are sintered and insulated for 3 hours at 1100 ℃ after being subjected to plastic removal at 650 ℃ to obtain the Ce-substituted modified bismuth titanium tantalate leadless piezoelectric ceramic. And polishing the surface of the obtained ceramic sample, coating an Ag electrode on the upper surface and the lower surface of the ceramic sample, polarizing for 30min in silicone oil at 180 ℃ under the direct current voltage of 12kV/mm, and testing the piezoelectric property of the ceramic sample. Piezoelectric constant d of the obtained ceramic sample3316pC/N, dielectric constant ∈ 102, dielectric loss tan δ 0.15%, electromechanical coupling coefficient kp11.2%, mechanical quality factor Qm＝12500。
CeO prepared in this example2The SEM scanning electron microscope picture of the substituted modified bismuth titanium tantalate lead-free piezoelectric ceramic is shown in figure 1.
Example 3:
preparation of Bi of chemical composition2.90Ce0.10TiTaO9And x is 0.10 of Ce substituted and modified bismuth titanium tantalate leadless piezoelectric ceramics.
Analytically pure powder raw material Bi2O3、TiO2、Ta2O5And CeO2The materials are proportioned according to the chemical proportion, the weighed raw materials are mixed with deionized water and then are ball-milled for 18h, pre-sintered for 3h at 800 ℃, crushed and then are ball-milled for 18h for the second time, the crushed materials are pressed into thin wafers with the diameter of 12mm after being dried and ground, and the thin wafers are sintered and insulated for 3h at 1100 ℃ after being subjected to plastic removal at 650 ℃ to obtain the doped and modified bismuth titanium tantalate leadless piezoelectric ceramic. And polishing the surface of the obtained ceramic sample, coating an Ag electrode on the upper surface and the lower surface of the ceramic sample, polarizing for 30min in silicone oil at 180 ℃ under the direct current voltage of 12kV/mm, and testing the piezoelectric property of the ceramic sample. Piezoelectric constant d of the obtained ceramic sample3313pC/N, dielectric constant ∈ 110, dielectric loss tan δ 0.35%, electromechanical coupling coefficient kp9.2%, mechanical quality factor Qm＝9800。
The formulation compositions and performance test results of the doped and modified bismuth titanium tantalate leadless piezoelectric ceramics of examples 1-3 are shown in Table 1.
TABLE 1 formulation compositions and performance test results for the substituted modified bismuth titantantalate lead-free piezoelectric ceramics of examples 1-3
Comparative example 1:
lead-free piezoelectric ceramic of unsubstituted modified bismuth titanium tantalate and its chemical composition Bi3TiTaO9The preparation method is the same as that of example 2, and the unsubstituted and modified bismuth titanium tantalate leadless piezoelectric ceramic is prepared. The piezoelectric performance was tested. Piezoelectric constant d of the obtained ceramic sample334pC/N, dielectric loss tan delta 1.1%, Curie temperature 890 ℃.
Comparative example 2:
adjusting the substitution element to La, the chemical composition of which is Bi2.95La0.05TiTaO9X is 0.05, prepared as in example 2, except that: la and La2O3Adding Ce in the form of CeO2Adding the powder to prepare the La substituted modifiedThe lead-free piezoelectric ceramic of bismuth titanium tantalate. The piezoelectric performance was tested. Piezoelectric constant d of the obtained ceramic sample3310pC/N, dielectric loss tan δ 0.32%, curie temperature 875 ℃.
The above description is only a preferred embodiment of the present disclosure and is not intended to limit the present disclosure, and various modifications and changes may be made to the present disclosure by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present disclosure should be included in the protection scope of the present disclosure.
Claims (12)
1. A bismuth titanium-tantalate high-temperature piezoelectric ceramic material with a bismuth layer structure is characterized in that: the general formula of the high-temperature piezoelectric ceramic material is Bi3-xCexTiTaO9Wherein x is more than 0 and less than or equal to 0.20.
2. The high temperature piezoceramic material according to claim 1, wherein: x is 0.02, 0.05, 0.1.
3. The preparation method of the bismuth titanium tantalate high-temperature piezoelectric ceramic material with the bismuth layer-structured as claimed in claim 1, is characterized in that: with Bi2O3Powder, TiO2Powder, Ta2O5Powder and CeO2The powder is taken as a raw material, and is prepared according to the stoichiometric ratio of Bi, Ti, Ta and Ce in the general formula, and is subjected to pre-ball milling to obtain mixed powder;
drying the mixed powder, and then performing presintering to obtain presintering powder;
performing secondary ball milling on the pre-sintered powder to obtain powder subjected to secondary ball milling;
adding a bonding agent into the powder subjected to the secondary ball milling to press the powder into ceramic blank sheets, and performing plastic removal treatment;
and sintering the ceramic blank sheet after the plastic removal treatment, and cooling to obtain the high-temperature piezoelectric ceramic material.
4. The production method according to claim 3, characterized in that: the ball milling medium of the pre-ball milling and the secondary ball milling is deionized water; the ball milling speed of the pre-ball milling and the secondary ball milling is 200-250 r/min.
5. The production method according to claim 3, characterized in that: the drying temperature of the mixed powder after the pre-ball milling is 100-120 ℃.
6. The production method according to claim 3, characterized in that: the pre-sintering temperature is 800-900 ℃, and the pre-sintering heat preservation time is 3-6 h.
7. The production method according to claim 3, characterized in that: the adhesive is 5 weight percent polyvinyl alcohol aqueous solution; the dosage of the adhesive is 6-8% of the total weight of the powder after the secondary ball milling.
8. The production method according to claim 3, characterized in that: the plastic discharge temperature is 600-700 ℃.
9. The production method according to claim 3, characterized in that: the sintering temperature is 1000-1200 ℃, and the sintering heat preservation time is 2-4 h; the sintering temperature rise rate is 4-6 ℃/min.
10. The method for preparing the high-temperature piezoelectric ceramic by using the high-temperature piezoelectric ceramic material prepared by the preparation method of any one of claims 3 to 9 comprises the following specific steps: polishing the high-temperature piezoelectric ceramic blank sheet, coating silver electrodes on the upper and lower surfaces of the blank sheet by a silver burning treatment method after polishing, and polarizing the blank sheet after silver burning treatment to obtain Bi with a bismuth layer structure3TiTaO9High temperature piezoelectric ceramics.
11. The method for preparing high-temperature piezoelectric ceramic by using the high-temperature piezoelectric ceramic material prepared by the preparation method as claimed in claim 10, wherein the silver firing treatment temperature is 500-600 ℃, and the heat preservation time of the silver firing treatment is 1-2 h.
12. The method for preparing high-temperature piezoelectric ceramic by using the high-temperature piezoelectric ceramic material prepared by the preparation method as claimed in claim 10, wherein the temperature of the polarization treatment is 150-.
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