CN109796205A - A kind of bismuth laminated titanium bismuth tantalate high temperature piezoceramics and preparation method thereof - Google Patents
A kind of bismuth laminated titanium bismuth tantalate high temperature piezoceramics and preparation method thereof Download PDFInfo
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Abstract
This disclosure relates to which a kind of bismuth laminated titanium bismuth tantalate high temperature piezoceramics and preparation method thereof, belong to high temperature piezoceramics technical field, the general formula of high temperature piezoceramics is Bi3‑xCexTiTaO9, wherein 0 x≤0.20 <.The preparation method comprises the following steps: with Bi2O3Powder, TiO2Powder, Ta2O5Powder and CeO2Powder be raw material by pre- ball milling, drying, sintering, secondary ball milling, prepare ceramic green sheet, plastic removal, sintering obtain high temperature piezoceramics, obtained blank is polished, make the upper and lower surface of blank by upper silver electrode by silver ink firing processing method after polishing, blank is polarised to obtain bismuth laminated Bi after silver ink firing processing3TiTaO9High-temperature piezoelectric ceramics.Piezoelectric constant d with 12-16pC/N33。
Description
Technical field
The disclosure belongs to high temperature piezoceramics technical field, and in particular to a kind of bismuth laminated titanium bismuth tantalate high temperature
Piezoceramic material and preparation method thereof.
Background technique
Disclosing the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, without certainty
It is considered as recognizing or implying in any form that information composition has become existing skill well known to persons skilled in the art
Art.
Piezoelectric ceramics is widely used in Industry Control, environmental monitoring, communication, letter as sensor, brake and frequency converter
The fields such as breath system and medical instrument.In piezoelectric ceramics field, the piezoelectric material being widely used at present mainly has calcium titanium
PZT (the PbZrO of mine structure3-PbTiO3) material.
However, PZT (PbZrO3-PbTiO3) material is leaded ceramics, wherein lead oxide (or lead orthoplumbate) accounts for about raw material
70% or so of gross mass.Leaded piezoelectricity ferro ceramics can all give environment and the mankind in processing, sintering process and use process
Bring harm.Therefore, exploitation the environment compatibility piezoceramic material without lead base be one it is urgent and have important scientific meaning
Project.
Currently, the leadless piezoelectric ceramics system studied both at home and abroad mainly has: barium titanate series, bismuth-sodium titanate system, alkali metal niobium
Phosphate-gallate series, bismuth laminated, tungsten bronze structure leadless piezoelectric ceramics.Wherein, bismuth laminated leadless piezoelectric ceramic material conduct
A kind of ferroelectric material has the characteristics that photoelectric effect, nonlinear optical effect, unusual photovoltaic effect, photorefractive effect, together
When there are also high Curie temperature, the advantages that polarization intensity is higher, good fatigue resistance and small leakage current and studied
The attention of person.But the piezoelectric property of bismuth laminated leadless piezoelectric ceramic is also not satisfactory.
Disclosure
For above-mentioned problems of the prior art, a purpose of the disclosure is to provide a kind of bismuth laminated titanium tantalum
Sour bismuth high temperature piezoceramics.
In order to solve the above technical problems, the technical solution of the disclosure are as follows:
A kind of bismuth laminated titanium bismuth tantalate high temperature piezoceramics, the general formula of high temperature piezoceramics are Bi3- xCexTiTaO9, wherein 0 x≤0.20 <.
In general formula, the molar ratio of index number representative element.
In some embodiments, x=0.02,0.05,0.1.
The bismuth laminated titanium bismuth tantalate high temperature piezoceramics have the piezoelectric constant d of 12-16pC/N33.Curie
Temperature is 870-885 DEG C, QmFor 8200-12500, QmReflect the mechanical loss ability of piezoelectric material, QmBigger mechanical loss is more
It is small, illustrate that the various aspects of performance of titanium bismuth tantalate high temperature piezoceramics made from the disclosure all preferably has preferable volume application
Property.
The disclosure the utility model has the advantages that
The bismuth laminated titanium bismuth tantalate high temperature piezoceramics of the disclosure, while not reducing its Curie temperature,
Its piezoelectric property is improved, is a kind of novel, environmentally friendly piezoceramic material.And preparation method simple process,
It is easy to operate, it is suitable for large-scale industrial production.
Detailed description of the invention
The Figure of description for constituting a part of this disclosure is used to provide further understanding of the present application, and the disclosure is shown
Meaning property embodiment and its explanation do not constitute the improper restriction to the disclosure for explaining the disclosure.
Fig. 1 is the SEM scanning electron microscope (SEM) photograph for the titanium bismuth tantalate piezoceramic material that Ce obtained replaces in the embodiment of the present disclosure 2
Piece.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the disclosure.Unless another
It indicates, all technical and scientific terms used herein has usual with disclosure person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Bismuth laminated ceramic material is by (Bi2O2)2+Layer and perovskite structure lattice layer alternate superposition and
At, chemical general formula is (Bi2O2)2+(Am-1BmO3m+1)2-, A is the ions for being suitble to 12 coordinations, such as Na in above formula+、K+、Ca2+
It is the ions for being suitble to 8 coordinations, such as Ti Deng, B4+、Nb5+Deng, m is integer, value be 1~5.Titanium bismuth tantalate (Bi3TiTaO9) it is m=
2 bismuth layer structure, Curie temperature is up to 890 DEG C, piezoelectric constant d33About 4pC/N, dielectric loss tan δ < 2%, with reality
Border is using comparing, although Curie temperature meets the requirement used under high temperature, application requirement is also not achieved in its piezoelectric property.Cause
How this, improve piezoelectric constant while not reducing Curie temperature to obtain the bismuth layered piezoelectric stablized in high temperature range and used
Ceramic material becomes an important topic of this field research.Bi is replaced to improve bismuth laminated titanium with Ce currently, yet there are no
The relevant report of bismuth tantalate high temperature piezoceramics performance, therefore, researching and developing the high temperature piezoceramics haveing excellent performance has
Great practical value.
In the titanium bismuth tantalate high temperature piezoceramics of the disclosure, Bi element is replaced by Ce element, and optimize doping
The additional amount of element effectively increases the piezoelectric property of titanium bismuth tantalate high temperature piezoceramics.It should be noted that existing skill
Although being different doped chemical, doping member there are many about the report for carrying out element doping to piezoceramic material in art
The different additional amount of element, can all produce bigger effect the overall performance of piezoceramic material, this is needed during the test not
Disconnected to grope, repetition test can just obtain, and inventor has also attempted a variety of different elements to titanium bismuth tantalate high temperature in early-stage study
The substitution of piezoceramic material, doping vario-property, but relative to other elements substitution, doping, replaced using Ce element of the invention
The bismuth laminated titanium bismuth tantalate high temperature piezoceramics that Bi element is prepared show more excellent piezoelectric property.
A kind of bismuth laminated titanium bismuth tantalate high temperature piezoceramics, the general formula of high temperature piezoceramics are Bi3- xCexTiTaO9, wherein 0 x≤0.20 <.
In general formula, the molar ratio of index number representative element.
In some embodiments, x=0.02,0.05,0.1.
A kind of preparation method of bismuth laminated titanium bismuth tantalate high temperature piezoceramics, specific steps are as follows:
With Bi2O3Powder, TiO2Powder, Ta2O5Powder and CeO2Powder is raw material, by the change of Bi, Ti, Ta and Ce in general formula
It learns metering and obtains mixed powder than carrying out ingredient, pre- ball milling；
The mixed powder is dried, is pre-sintered again after drying, the powder by pre-sintering is obtained；
The powder by being pre-sintered is subjected to secondary ball milling, obtains the powder by secondary ball milling；
Compressed with adhesive is added into the powder by secondary ball milling into ceramic green sheet, and carries out plastic removal processing；
By plastic removal, treated that ceramic green sheet is sintered, and cooling obtains high temperature piezoceramics.
In some embodiments, the ball-milling medium of the pre- ball milling and secondary ball milling is deionized water.
The dosage of deionized water is the 80-100% of the raw material gross weight.In the present invention, deionized water is as raw material
Bi2O3、TiO2、Ta2O5And CeO2Solvent, and the additional amount of deionized water is optimized, can under dosage of the invention
To meet the abundant ball milling to raw material.
In some embodiments, the ball milling speed of the pre- ball milling and secondary ball milling is 200-250r/min.
The time of ball milling is 12-24h.The ball milling speed and Ball-milling Time can be by the abundant ball millings of raw material to centainly thin
Degree, is conducive to the compacting of subsequent ceramic green sheet.
In some embodiments, the drying temperature of the mixed powder after pre- ball milling is 100-120 DEG C；.
Mixed powder is dried at such a temperature, and main purpose is the deionized water added in the pre- ball milling of removal.
In some embodiments, pre-sintering temperature is 800-900 DEG C, and the soaking time of pre-sintering is 3-6h.
Pre-sintering temperature and soaking time is optimized in the present invention, under this condition, has above-mentioned lead to be made
The high temperature piezoceramics of formula composition, and by being pre-sintered, it can also further improve titanium bismuth tantalate high-temperature piezoelectric ceramics
The temperature stability of the piezoelectric property of material.
In some embodiments, described adhesive is the polyvinyl alcohol water solution that weight percentage is 5%.
In some embodiments, the dosage of adhesive is the 6-8% of powder total weight after secondary ball milling.
Mixed powder can be made sufficiently to bond using the adhesive of the dosage.
In some embodiments, the plastic removal temperature is 600-700 DEG C.
In some embodiments, the sintering temperature is 1000-1200 DEG C, and the sintered heat insulating time is 2-4h.
In the present invention, control the sintering temperature, can be conducive to titanium bismuth tantalate high temperature piezoceramics formed it is single-phase
Structure.
In some embodiments, the sintering heating rate is 4-6 DEG C/min.
In the disclosure, the heating rate of sintering is effectively controlled, it is ensured that the integrality of ceramic green sheet, if heated up
It may result in the rupture of ceramic green sheet fastly.
A kind of preparation method of bismuth laminated titanium bismuth tantalate high-temperature piezoelectric ceramics, specific steps are as follows:
High-temperature piezoelectric ceramic green sheet obtained above is polished, the upper of blank is made by silver ink firing processing method after polishing
Lower surface is polarised blank to obtain bismuth laminated Bi by upper silver electrode after silver ink firing processing3TiTaO9High-temperature piezoelectric pottery
Porcelain.
In some embodiments, the silver ink firing treatment temperature is 500-600 DEG C, and it is 1-2h that silver ink firing, which handles soaking time,.
In some embodiments, the temperature of the polarization process is 150-200 DEG C, and polarized voltage is 10-12kV/mm,
The polarized time is 20-40min.
Under the conditions of the polarization process, the bismuth laminated titanium bismuth tantalate high temperature piezoceramics that Ce element replaces, energy
Sufficiently polarization, improves its piezoelectric property.
The disclosure is further illustrated below with reference to embodiment
Embodiment 1:
Preparation meets chemical composition Bi2.98Ce0.02TiTaO9, the titanium bismuth tantalate leadless piezoelectric of the Ce substituting modification of x=0.02
Ceramics.
By analytically pure powder material Bi2O3、TiO2、Ta2O5And CeO2It, will be load weighted according to the above stoicheiometry ingredient
Ball milling 12h after raw material is mixed with deionized water, it is pressed after 850 DEG C of pre-burning 3h, secondary ball milling 12h after crushing, drying grinding
The thin discs of diameter 12mm are made, sintered heat insulating 3h obtains the titanium tantalum of Ce substituting modification at 1100 DEG C after 650 DEG C of plastic removals
Sour bismuth leadless piezoelectric ceramics.By lower surface is by upper Ag electrode on it after resulting ceramics sample surface polishing, in 200 DEG C of silicone oil
In, polarize 30min under the DC voltage of 12kV/mm, tests its piezoelectric property.The piezoelectric constant d of gained ceramics sample33=
12pC/N, permittivity ε=98, dielectric loss tan δ=0.2%, electromechanical coupling factor kp=8.5%, mechanical quality factor Qm
=8200.
Embodiment 2:
Preparation meets chemical composition Bi2.95Ce0.05TiTaO9, the titanium bismuth tantalate leadless piezoelectric of the Ce substituting modification of x=0.05
Ceramics.
By analytically pure powder material Bi2O3、TiO2、Ta2O5And CeO2It, will be load weighted according to the above stoicheiometry ingredient
Ball milling 12h after raw material is mixed with deionized water, it is pressed after 850 DEG C of pre-burning 3h, secondary ball milling 12h after crushing, drying grinding
The thin discs of diameter 12mm are made, sintered heat insulating 3h obtains the titanium tantalum of Ce substituting modification at 1100 DEG C after 650 DEG C of plastic removals
Sour bismuth leadless piezoelectric ceramics.By lower surface is by upper Ag electrode on it after resulting ceramics sample surface polishing, in 180 DEG C of silicone oil
In, polarize 30min under the DC voltage of 12kV/mm, tests its piezoelectric property.The piezoelectric constant d of gained ceramics sample33=
16pC/N, permittivity ε=102, dielectric loss tan δ=0.15%, electromechanical coupling factor kp=11.2%, mechanical quality because
Number Qm=12500.
CeO manufactured in the present embodiment2The SEM scanning electron microscopic picture of the titanium bismuth tantalate leadless piezoelectric ceramics of substituting modification is shown in figure
1。
Embodiment 3:
Preparation meets chemical composition Bi2.90Ce0.10TiTaO9, the titanium bismuth tantalate leadless piezoelectric of the Ce substituting modification of x=0.10
Ceramics.
By analytically pure powder material Bi2O3、TiO2、Ta2O5And CeO2It, will be load weighted according to the above stoicheiometry ingredient
Ball milling 18h after raw material is mixed with deionized water, it is pressed after 800 DEG C of pre-burning 3h, secondary ball milling 18h after crushing, drying grinding
The thin discs of diameter 12mm are made, sintered heat insulating 3h obtains the titanium tantalic acid of doping vario-property at 1100 DEG C after 650 DEG C of plastic removals
Bismuth leadless piezoelectric ceramics.By lower surface is by upper Ag electrode on it after resulting ceramics sample surface polishing, in 180 DEG C of silicone oil
In, polarize 30min under the DC voltage of 12kV/mm, tests its piezoelectric property.The piezoelectric constant d of gained ceramics sample33=
13pC/N, permittivity ε=110, dielectric loss tan δ=0.35%, electromechanical coupling factor kp=9.2%, mechanical quality factor
Qm=9800.
The formula composition and the performance test results of the titanium bismuth tantalate leadless piezoelectric ceramics of the doping vario-property of embodiment 1-3 are specific
It is shown in Table 1.
The formula composition and the performance test results of the titanium bismuth tantalate leadless piezoelectric ceramics of the substituting modification of 1 embodiment 1-3 of table
Comparative example 1:
The titanium bismuth tantalate leadless piezoelectric ceramics of unsubstituted modification, chemical composition Bi3TiTaO9, the same embodiment of preparation method
2, the titanium bismuth tantalate leadless piezoelectric ceramics of unsubstituted modification is prepared.Test its piezoelectric property.The piezoelectricity of gained ceramics sample
Constant d33=4pC/N, dielectric loss tan δ=1.1%, Curie temperature are 890 DEG C.
Comparative example 2:
Substitution element is adjusted to La, chemical composition Bi2.95La0.05TiTaO9, x=0.05, the same embodiment of preparation method
2, difference is: La is with La2O3The form of powder is added, and Ce is with CeO2The form of powder is added, and La substituting modification is prepared
Titanium bismuth tantalate leadless piezoelectric ceramics.Test its piezoelectric property.The piezoelectric constant d of gained ceramics sample33=10pC/N, dielectric loss
Tan δ=0.32%, Curie temperature are 875 DEG C.
The foregoing is merely preferred embodiment of the present disclosure, are not limited to the disclosure, for the skill of this field
For art personnel, the disclosure can have various modifications and variations.It is all within the spirit and principle of the disclosure, it is made any to repair
Change, equivalent replacement, improvement etc., should be included within the protection scope of the disclosure.
Claims (10)
1. a kind of bismuth laminated titanium bismuth tantalate high temperature piezoceramics, it is characterised in that: high temperature piezoceramics lead to
Formula is Bi3-xCexTiTaO9, wherein 0 x≤0.20 <.
2. high temperature piezoceramics according to claim 1, it is characterised in that: x=0.02,0.05,0.1.
3. a kind of preparation method of bismuth laminated titanium bismuth tantalate high temperature piezoceramics, it is characterised in that: with Bi2O3Powder,
TiO2Powder, Ta2O5Powder and CeO2Powder is raw material, carries out ingredient by the stoichiometric ratio of Bi, Ti, Ta and Ce in general formula, in advance
Ball milling obtains mixed powder；
The mixed powder is dried, is pre-sintered again after drying, the powder by pre-sintering is obtained；
The powder by being pre-sintered is subjected to secondary ball milling, obtains the powder by secondary ball milling；
Compressed with adhesive is added into the powder by secondary ball milling into ceramic green sheet, and carries out plastic removal processing；
By plastic removal, treated that ceramic green sheet is sintered, and cooling obtains high temperature piezoceramics.
4. preparation method according to claim 3, it is characterised in that: the ball-milling medium of the pre- ball milling and secondary ball milling is
Deionized water；The ball milling speed of the pre- ball milling and secondary ball milling is 200-250r/min.
5. preparation method according to claim 3, it is characterised in that: the drying temperature of the mixed powder after pre- ball milling is
100-120℃。
6. preparation method according to claim 3, it is characterised in that: pre-sintering temperature is 800-900 DEG C, the guarantor of pre-sintering
The warm time is 3-6h.
7. preparation method according to claim 3, it is characterised in that: described adhesive is that weight percentage is 5%
Polyvinyl alcohol water solution；The dosage of adhesive is the 6-8% of powder total weight after secondary ball milling.
8. preparation method according to claim 3, it is characterised in that: the plastic removal temperature is 600-700 DEG C.
9. preparation method according to claim 3, it is characterised in that: the sintering temperature is 1000-1200 DEG C, and sintering is protected
The warm time is 2-4h；Sintering heating rate is 4-6 DEG C/min.
10. preparing high temperature using the high temperature piezoceramics that the described in any item preparation methods of claim 3-9 are prepared
The method of piezoelectric ceramics, specific steps are as follows: high-temperature piezoelectric ceramic green sheet is processed by shot blasting, passes through silver ink firing processing side after polishing
Method makes the upper and lower surface of blank by upper silver electrode, is polarised to obtain to blank after silver ink firing processing bismuth laminated
Bi3TiTaO9High-temperature piezoelectric ceramics；
Preferably, the silver ink firing treatment temperature is 500-600 DEG C, and it is 1-2h that silver ink firing, which handles soaking time,；
Preferably, the temperature of the polarization process is 150-200 DEG C, and polarized voltage is 10-12kV/mm, and the polarized time is
20-40min。
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Cited By (5)
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| CN112023912A (en) * | 2020-08-31 | 2020-12-04 | 陕西科技大学 | Bismuth-based photocatalyst loaded with elemental bismuth and preparation method and application thereof |
| CN113321500A (en) * | 2021-06-30 | 2021-08-31 | 山东大学 | High Curie temperature piezoelectric ceramic and preparation method thereof |
| CN113683410A (en) * | 2021-08-09 | 2021-11-23 | 中国科学院上海硅酸盐研究所 | Bismuth titanate-based bismuth layer-structured lead-free piezoelectric ceramic with negative charge-trapping effect and preparation method thereof |
| CN113956034A (en) * | 2021-11-12 | 2022-01-21 | 中国电子科技集团公司第四十六研究所 | Method for preparing sodium bismuth titanate piezoelectric ceramic by adopting low-granularity powder |
| CN117326868A (en) * | 2023-12-02 | 2024-01-02 | 山东利恩斯智能科技有限公司 | Ceramic material, preparation method thereof and application thereof in piezoelectricity |
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| CN113683410A (en) * | 2021-08-09 | 2021-11-23 | 中国科学院上海硅酸盐研究所 | Bismuth titanate-based bismuth layer-structured lead-free piezoelectric ceramic with negative charge-trapping effect and preparation method thereof |
| CN113956034A (en) * | 2021-11-12 | 2022-01-21 | 中国电子科技集团公司第四十六研究所 | Method for preparing sodium bismuth titanate piezoelectric ceramic by adopting low-granularity powder |
| CN117326868A (en) * | 2023-12-02 | 2024-01-02 | 山东利恩斯智能科技有限公司 | Ceramic material, preparation method thereof and application thereof in piezoelectricity |
| CN117326868B (en) * | 2023-12-02 | 2024-02-13 | 山东利恩斯智能科技有限公司 | Ceramic material, preparation method thereof and application thereof in piezoelectricity |
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