CN104725045B - Bismuth laminar-structure piezoelectric ceramic and preparation method thereof, method for enhancing high-temperature resistivity of bismuth laminar-structure piezoelectric ceramic - Google Patents
Bismuth laminar-structure piezoelectric ceramic and preparation method thereof, method for enhancing high-temperature resistivity of bismuth laminar-structure piezoelectric ceramic Download PDFInfo
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Abstract
The invention relates to a bismuth laminar-structure piezoelectric ceramic and a preparation method thereof, a method for enhancing high-temperature resistivity of the bismuth laminar-structure piezoelectric ceramic. The bismuth laminar-structure piezoelectric ceramic comprises a main phase and high-insulation-resistance oxide powder granules as a second phase, wherein the main phase comprises Na0.5Bi2.5Nb2O9, Bi3TiNbO9, CaBi2Nb2O9 and/or Bi4Ti3O12; and the weight ratio of the second phase to the main phase is less than or equal to 10%, preferably 1-5%. According to the new method provided by the invention, oxides are doped at the grain boundary to form the second phase and regulate the microstructure, thereby effectively enhancing the high-temperature resistivity of the bismuth laminar-structure piezoelectric ceramic, synergically optimizing the dielectric property and piezoelectricity, and providing a new way for preparing the bismuth laminar-structure piezoelectric ceramic for high-temperature piezoelectric vibration sensors.
Description
Technical field
The invention belongs to the preparation field of piezoceramic material, is related to a kind of higher bismuth stratiform knot of resistivity at high temperature
Structure piezoelectric ceramics and preparation method thereof.
Background technology
Piezoceramic material is the extremely important functional material of a class for realizing machine-electric energy conversion and coupling, in aviation
The fields such as space flight, electronic information, the energy, advanced manufacture, medical system and weaponry are widely used.In recent years, China
Develop very rapidly in fields such as Aero-Space, the energy, medical treatment and space technologies, wherein key feature is proposed more next
Harsher requirement.Pass in piezoelectric device such as acoustic logging instrument, ultrasound electric machine, the high-temperature piezoelectric vibration of some key areas applications
One common feature of sensor etc. is exactly that operating ambient temperature is high, and this requires piezoceramic material stablize at high temperature, can
The work leaned on.
Piezoceramic material is the core parts of high-temperature vibrating sensor.Laminated structure bismuth piezoelectric ceramic material is due to Curie
Temperature higher (650～970 DEG C), dielectric loss is relatively low and resistivity is higher, is current 482 DEG C of high-temperature piezoelectric vibrating sensors
With the unique technical scheme of high temperature piezoceramics.But drastically decline as its resistivity is raised with temperature, leakage current increase,
Dependent piezoelectric component failure is directly resulted in, seriously constraining laminated structure bismuth piezoelectric ceramic material reality in high temperature environments should
One of with, and the bottleneck that not yet makes a breakthrough of the development of 482 DEG C of high-temperature piezoelectric vibrating sensors of China.
At present, the means such as ion doping optimization composition commonly employed in the art design and texture techniques regulation and control micro structure
To improve the high-temperature resistivity of laminated structure bismuth piezoelectric ceramic material.Such as pass through W6+Donor doping replaces can will be bismuth laminated
Bi3TiNbO9And Na0.5Bi2.5Nb2O9The resistivity of piezoelectric ceramics improve 2～3 orders of magnitude (J.Appl.Phys., 100,
2006:044112；Appl.Phys.Lett.,104,2014:012904)；Micro structure is regulated and controled by texturing forge hot sintering process
Afterwards, Bi can be made3TiNbO9Piezoelectric ceramics is higher by 1～2 order of magnitude in the axial resistivity ratio vertical direction of parallel forge hot.But
It is, due to the performance often mutually restriction, interactional of piezoceramic material.Ion doping replacement can improve piezoelectric ceramics
The resistivity of material, but while the Curie temperature even piezoelectric moduluses that can also reduce material (evaluate piezoceramic material performance
Two other important parameter)；And the texture techniques such as means such as hot pressing, forge hot, rapid plasma sintering, technique is more multiple
Miscellaneous, repeatability is poor.Therefore, how while laminated structure bismuth piezoelectric ceramic material high-curie temperature is kept, collaboration is improved
Its high-temperature resistivity, is the research emphasis and crucial problem in high-temperature piezoelectric ceramic applications field.
The content of the invention
It is contemplated that overcome existing laminated structure bismuth piezoelectric ceramic material performance deficiency under the high temperature conditions, the present invention
There is provided a kind of laminated structure bismuth piezoelectric ceramic and preparation method thereof.
A kind of laminated structure bismuth piezoelectric ceramic with high resistivity under high temperature, wherein, the bismuth laminated piezoelectricity pottery
Porcelain includes principal phase and the oxide powder granule with high insulation resistance as the second phase, wherein, principal phase includes
Na0.5Bi2.5Nb2O9、Bi3TiNbO9、CaBi2Nb2O9And/or Bi4Ti3O12, second with the weight ratio≤10% of principal phase, preferably
Between 1～5%.
It is preferred that the oxide powder granule with high insulation resistance is Al2O3Powder granule.
It is preferred that described second is mutually formed at the grain boundaries of principal phase, do not enter in the lattice of principal phase.
Present invention also offers a kind of preparation method of above-mentioned laminated structure bismuth piezoelectric ceramic, including：
1) constitute by the laminated structure bismuth piezoelectric ceramic principal phase, weigh corresponding oxidation raw material respectively, Jing uniformly mixes
Afterwards, synthesize at 650～900 DEG C, obtain the piezoelectric ceramic powder that principal phase material is composition；
2) by the second phase composition of the laminated structure bismuth piezoelectric ceramic, corresponding oxidation raw material is weighed, will be with principal phase material
For the piezoelectric ceramic powder and the second phase oxide powder body of composition, it is uniform mix after as material powder；
3) material powder is carried out into forming processes, forms the base substrate of the laminated structure bismuth piezoelectric ceramic；
4) base substrate is sintered at 1000～1200 DEG C and obtains the laminated structure bismuth piezoelectric ceramic.
The present invention also provide it is a kind of improve laminated structure bismuth piezoelectric ceramic at a high temperature of resistivity method, wherein described
Method includes piling up using the particles filled laminated structure bismuth piezoelectric ceramic sheet-like particle of oxide powder with high insulation resistance
The space of formation or pore, the weight of the oxide powder granule and laminated structure bismuth piezoelectric ceramic sheet-like particle than≤
10%.
It is preferred that preparing using solid reaction process, the oxide powder granule with high insulation resistance is added to into synthesis
In laminated structure bismuth piezoelectric ceramic sheet-like particle afterwards, then modified laminated structure bismuth piezoelectric ceramic is prepared by molding, sintering,
The modified laminated structure bismuth piezoelectric ceramic does not add the bismuth layer of the oxide powder granule with high insulation resistance relatively
Shape structure piezoelectric ceramics, under high temperature, resistivity improves 1～3 order of magnitude.
Beneficial effects of the present invention：
The invention discloses a kind of method for improving laminated structure bismuth piezoelectric ceramic high-temperature resistivity.Using with high insulation
The particles filled laminated structure bismuth piezoelectric ceramic of oxide powder (consisting of principal phase material in the present invention) the sheet-like particle heap of resistance
Space or pore that product is formed, during solid reaction process prepares ceramic material, the oxidate powder with high insulation resistance
Body is added in the piezoelectric ceramic powder after synthesis, and the bismuth layer of oxide modifying is then prepared by techniques such as molding, sintering
Shape structure piezoelectric ceramics；Using new method proposed by the present invention, form the second phase, regulate and control micro- in grain boundaries by oxide-doped
Structure, while laminated structure bismuth piezoelectric ceramic high-temperature resistivity is effectively improved can cooperate with and optimize its dielectric and piezoelectricity
Can, meet high-temperature piezoelectric vibrating sensor laminated structure bismuth piezoelectric ceramic and provide new way to prepare.
Description of the drawings
Fig. 1 shows the platelet grain morphology schematic diagram of the piezoelectric ceramics with principal phase material to constitute；
Fig. 2 shows signal of the second phase filler particles in principal phase material in laminated structure bismuth piezoelectric ceramic of the invention
Figure；
Fig. 3 shows different Al2O3Doping is modified Na0.5Bi2.5Nb2O9The natural surface pattern (SEM) of ceramics；
Fig. 4 shows different Al2O3Doping is modified Na0.5Bi2.5Nb2O9The high-temperature resistivity variation with temperature of ceramics
Figure.
Specific embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and following embodiments, it should be appreciated that accompanying drawing and following embodiments
It is merely to illustrate the present invention, and the unrestricted present invention.
In order to, while laminated structure bismuth piezoelectric ceramic material high-curie temperature is kept, collaboration improves its high temperature resistance
Rate, the invention provides a kind of fill the method that flaky crystalline grain piles up space using with high insulation resistance oxide particle, carries
The resistivity of high (principal phase material is composition with the present invention) laminated structure bismuth piezoelectric ceramic material, is shaken with meeting high-temperature piezoelectric
The requirement of dynamic sensor high temperature piezoceramics, is that laminated structure bismuth piezoelectric ceramic material is played in the application of high-temperature field
Progradations.
Generally, the crystal grain of (principal phase material is composition with the present invention) laminated structure bismuth piezoelectric ceramic has typical big
Blade diameter length ratio sheet-like morphology feature.In sintering process, as flaky crystalline grain random orientation is arranged, easily formed in many grain boundaries and piled up
Space (or pore), as shown in Figure 1.These spaces or pore, on the one hand reduce the consistency of material, make pottery in polarization process
Porcelain can not apply high voltage (otherwise can be breakdown), lead to not fully inspire the piezoelectric property of ceramics；On the other hand meeting
Electric leakage circulation road is formed, so as to reduce the resistivity of ceramics.
Therefore, the present invention propose it is a kind of using the oxide particle with high insulation resistance fill above-mentioned accumulation space or
The method of pore, as shown in Fig. 2 mutually regulate and control micro structure by forming second in grain boundaries, improve the consistency of ceramic material with
And the formation of obstruction current channel, and then improve resistivity.By regulating and controlling suitable doping, second can be made mutually to be formed only in crystalline substance
At boundary, and do not enter in the lattice of piezoceramic material, while second is mutually non-ferroelectric phase, therefore Jie to piezoelectric ceramics
Electricity, ferroelectricity and piezoelectric property do not produce significant impact.The raising of resistivity is additionally, since, the institute when polarizing to ceramic material
The voltage of applying also accordingly can be improved, therefore piezoelectric ceramics can be made fully to be polarized, and piezoelectric property is improved.
The method comprises the steps：
Laminated structure bismuth piezoelectric ceramic is prepared using solid reaction process.In preparation process, the oxidation with high insulation resistance
Powder be added to synthesis after piezoelectric ceramic powder in (synthesis of piezoelectric ceramic powder adopts solid reaction process, can specifically join
Examine J.Appl.Phys., 100,2006:044112) the bismuth layer of oxide modifying, is then prepared by techniques such as molding, sintering
Shape structure piezoelectric ceramics, wherein, the oxide with high insulation resistance is Al2O3Powder body, Al2O3The addition and piezoelectricity of powder body
The weight ratio of ceramic powder is 0.0%～10%.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only that an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
Al is prepared for using solid reaction process2O3The bismuth laminated Na of doping0.5Bi2.5Nb2O9Piezoelectric ceramics.Wherein,
Al2O3The purity of powder material is 99.95%, and its addition is Na0.5Bi2.5Nb2O9The 1.0% of piezoelectric ceramic powder body weight, plus
Entering mode is and the Na after synthesis0.5Bi2.5Nb2O9Powder body fine grinding together, then (1150 DEG C of sintering temperature is burnt for Jing molding, sintering
Knot time 2 h, 3 DEG C/min of heating rate) etc. technique make.
Embodiment 2
Al is prepared for using solid reaction process2O3The bismuth laminated Na of doping0.5Bi2.5Nb2O9Piezoelectric ceramics.Wherein,
Al2O3The purity of powder material is 99.95%, and its addition is Na0.5Bi2.5Nb2O9The 3.0% of piezoelectric ceramic powder body weight, plus
Entering mode is and the Na after synthesis0.5Bi2.5Nb2O9Powder body fine grinding together, then (1150 DEG C of sintering temperature is burnt for Jing molding, sintering
Knot time 2 h, 3 DEG C/min of heating rate) etc. technique make.
Embodiment 3
Al is prepared for using solid reaction process2O3The bismuth laminated Na of doping0.5Bi2.5Nb2O9Piezoelectric ceramics.Wherein,
Al2O3The purity of powder material is 99.95%, and its addition is Na0.5Bi2.5Nb2O9The 5.0% of piezoelectric ceramic powder body weight, plus
Entering mode is and the Na after synthesis0.5Bi2.5Nb2O9Powder body fine grinding together, then (1160 DEG C of sintering temperature is burnt for Jing molding, sintering
Knot time 2 h, 3 DEG C/min of heating rate) etc. technique make.
Fig. 3 is difference Al2O3Doping is modified Na0.5Bi2.5Nb2O9The natural surface pattern of ceramics, it can be seen that in crystalline substance
The second phase is defined at boundary, the effect of filling space and pore is served, while grain boundaries little crystal grain shape is gradually become by lamellar
Glomeration, is conducive to improving consistency；On the other hand, these Second Phase Particles in grain boundaries also have obstruction current channel
Effect, be conducive to improve resistivity.
Fig. 4 is difference Al2O3Doping is modified Na0.5Bi2.5Nb2O9The high-temperature resistivity of ceramics, it can be seen that
Al2O3After doping, Na0.5Bi2.5Nb2O9The resistivity of ceramics improves two orders of magnitude, has reached 10 at 500 DEG C8Ω×cm
Magnitude.Further, since resistivity is greatly improved, in polarization process, the polarizing voltage of applying also accordingly increases, and piezoelectric property exists
More sufficiently eject under high voltage, therefore, Na0.5Bi2.5Nb2O9The piezoelectric coefficient d of ceramic material33Also have and significantly carry
It is high；Simultaneously as second is mutually non-ferroelectric phase, do not enter in ceramic material lattice yet, therefore to dielectric properties such as Curie's temperature
Degree is no to be affected, as shown in table 1.
1 difference Al of table2O3Doping is modified Na0.5Bi2.5Nb2O9The performance parameter contrast of ceramics
Can be seen that using new method proposed by the present invention, by Al from above-mentioned experimental result2O3It is entrained in grain boundaries
The second phase, regulation and control micro structure are formed, Na can effectively improved0.5Bi2.5Nb2O9While piezoelectric ceramics high-temperature resistivity, collaboration
Optimize its dielectric and piezoelectric properties, meet high-temperature piezoelectric vibrating sensor and provided with laminated structure bismuth piezoelectric ceramic to prepare
New way.
Claims (5)
1. a kind of laminated structure bismuth piezoelectric ceramic with high resistivity under high temperature, it is characterised in that the bismuth laminated pressure
Electroceramics includes principal phase and the oxide powder granule with high insulation resistance as the second phase, wherein, principal phase includes
Na0.5Bi2.5Nb2O9、Bi3TiNbO9、CaBi2Nb2O9And/or Bi4Ti3O12, second with the weight ratio of principal phase between 1～5%,
Described second grain boundaries for being mutually formed at principal phase, do not enter in the lattice of principal phase, the oxide powder with high insulation resistance
Grain is Al2O3Powder granule.
2. the preparation method of laminated structure bismuth piezoelectric ceramic described in a kind of claim 1, it is characterised in that include：
1）Constitute by the laminated structure bismuth piezoelectric ceramic principal phase, weigh corresponding oxidation raw material respectively, Jing after uniform mixing,
Synthesize at 650～900 DEG C, obtain the piezoelectric ceramic powder that principal phase material is composition；
2）By the second phase composition of the laminated structure bismuth piezoelectric ceramic, corresponding oxidation raw material is weighed, will be with principal phase material as group
Into piezoelectric ceramic powder and the second phase oxide powder body, it is uniform mix after as material powder；
3）Material powder is carried out into forming processes, the base substrate of the laminated structure bismuth piezoelectric ceramic is formed；
4）Base substrate is sintered at 1000～1200 DEG C and obtains the laminated structure bismuth piezoelectric ceramic.
3. it is a kind of improve laminated structure bismuth piezoelectric ceramic at a high temperature of resistivity method, it is characterised in that methods described bag
Include and pile up what is formed using the particles filled laminated structure bismuth piezoelectric ceramic sheet-like particle of oxide powder with high insulation resistance
Space or pore, the weight ratio of the oxide powder granule and laminated structure bismuth piezoelectric ceramic sheet-like particle 1～5% it
Between, the oxide powder granule with high insulation resistance is Al2O3Powder granule.
4. method according to claim 3, it is characterised in that the oxide powder granule is mutually formed at work as second
For the grain boundaries of the laminated structure bismuth piezoelectric ceramic sheet-like particle of principal phase.
5. method according to claim 3, it is characterised in that prepared using solid reaction process, will be with high insulation resistance
Oxide powder granule be added to synthesis after laminated structure bismuth piezoelectric ceramic powder body in, then by molding, sintering preparation change
Property laminated structure bismuth piezoelectric ceramic, the modified laminated structure bismuth piezoelectric ceramic is not added relatively described has high insulation resistance
Oxide powder granule laminated structure bismuth piezoelectric ceramic, under high temperature resistivity improve 1～3 order of magnitude.
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| CN113979741B (en) * | 2021-10-22 | 2022-08-19 | 厦门乃尔电子有限公司 | Bismuth layer-structured composite high-temperature piezoelectric ceramic material and preparation method thereof |
| CN114560698B (en) * | 2022-04-15 | 2023-04-07 | 中国科学院合肥物质科学研究院 | Method for enhancing performance of calcium bismuth niobate high-temperature piezoelectric ceramic by inducing texture through oxide sintering aid |
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| CN101186497B (en) * | 2007-12-07 | 2010-05-19 | 华南理工大学 | Method for increasing bismuth layer structure piezoelectricity ferroelectric ceramic material high-temperature resistivity |
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