CN105645955B - The preparation method of Tetragonal titanium magnesium acid bismuth lead titanate piezoelectric ceramics - Google Patents
The preparation method of Tetragonal titanium magnesium acid bismuth lead titanate piezoelectric ceramics Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of Tetragonal titanium magnesium acid bismuth lead titanate piezoelectric ceramics, the constitutional chemistry formula of the Tetragonal titanium magnesium acid bismuth lead titanate piezoelectric ceramics is (1x)Bi(Mg1/ 2Ti1/2)O3 ‑xPbTiO3, methods described includes：1）Weigh metal oxide powder；2）First by step 1）Weigh progress forming processes after metal oxide powder uniformly mixes and obtain piezoelectric ceramics biscuit, piezoelectric ceramics biscuit is then obtained into block ceramic in 1,000 1200 DEG C of sintering；3）By step 2）The block ceramic of preparation is covered with silver electrode or platinum electrode, and polarization process is carried out in silicone oil.
Description
Technical field
The present invention relates to a kind of preparation method of piezoelectric ceramics, and in particular to a kind of Tetragonal titanium magnesium acid bismuth-lead titanate
The preparation method of high-temperature piezoelectric ceramics.
Background technology
Piezoelectric can realize the mutual conversion between mechanical energy and electric energy, be a kind of important functional material, extensively
It is to form wave filter, transducing applied to numerous areas such as aviation, the energy, automobile making, communication, household electrical appliances, detection and computers
The important component of the electronic components such as device, sensor, piezoelectric transformer, it has also become the main direction of studying of 21 century new and high technology it
One.In recent ten years, with the rapid hair of the industry such as space flight and aviation, petrochemical industry, geological prospecting, nuclear energy power generation, automobile making
Exhibition, electronic equipment is needed to work at higher temperatures, while higher requirement is also proposed to piezoelectric, does not require nothing more than pressure
Electric material has excellent performance, but also requires that piezoelectric has higher temperature in use.Such as in car aircraft bonnet
Vibrating sensor, the piezoelectric on granule surface contral and Dynamic fuel injection nozzle require that operating temperature is up to 300 DEG C, oil well
The lower sound wave well logging transducer operating temperature used also reaches 200-300 DEG C.Therefore, many application requirements pressures now in the industry
Electric material must at a higher temperature (400 DEG C of ﹥) to occur without structural phase transition to ensure high temperature depolarization phenomenon does not occur and bad
Change the temperature stability of piezoelectric device.
Studying more temperature high performance high piezoelectric at present has scandium acid bismuth-lead titanates system and titanium magnesium acid bismuth lead titanates etc.
System.But the price and its costliness that prepare raw material scandium oxide of scandium acid bismuth-lead titanates, so that scandium acid bismuth-lead titanates
It is difficult to industrially obtain large-scale application.Titanium magnesium acid bismuth-lead titanates system piezoelectric ceramics is in document and patent
(C.A.Randall,R.E.Eitel,B.Jones,and T.R.Shrout,J Appl Phys,2004,95,3633；
Q.Zhang,Z.Li,F.Li,Z.Xu,and X.Yao,J Am Ceram Soc,2010,93,3330；CN 102336567A) in
Report.But its composition all concentrate on standard with phase boundary around, i.e. (1-x) Bi (Mg1/2Ti1/2)O3-xPbTiO3Middle x's
Value is less than 0.42, and its thing is mutually tripartite's phase, and the Curie temperature undoped with sample is below 450 DEG C, although having after doping manganese
Improved, but the amplitude improved is little, only 520 DEG C or so.It also is difficult to meet many high-temperature fields to materials'use temperature
Requirement.
The content of the invention
It is contemplated that it is difficult the performance deficiency for bearing high temperature to overcome existing titanium magnesium acid bismuth lead titanates system piezoelectric ceramics, this
Invention, which provides, a kind of undergoes after high temperature still Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectric ceramics with higher pressure electrical property
Preparation method.
The invention provides a kind of preparation method of Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectric ceramics, the Tetragonal
The constitutional chemistry formula of titanium magnesium acid bismuth-lead titanate piezoelectric ceramics is (1-x) Bi (Mg1/2Ti1/2)O3-xPbTiO3, wherein 0.50≤x
≤ 0.90, methods described includes：
1) mole in the Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectric ceramics constitutional chemistry formula between metallic element is pressed
Than, metal oxide powder is weighed, wherein, Bi oxide is Bi2O3, Mg oxide is MgO, and Ti oxide is TiO2,
Pb oxide is PbO and/or Pb3O4；
2) step 1) is first weighed into progress forming processes after metal oxide powder uniformly mixes and obtains piezoelectric ceramics biscuit,
Then piezoelectric ceramics biscuit is obtained into block ceramic in 1000-1200 DEG C of sintering；
3) block ceramic prepared by step 2) is covered with silver electrode or platinum electrode, polarization process is carried out in silicone oil.
It is preferred that 0.55≤x≤0.70.
It is preferred that 0.58≤x≤0.64.
It is used to adulterate Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectricity it is preferred that in the metal oxide powder also containing
The MnO of ceramics2、Cr2O3、CuO、Nb2O5、La2O3, NiO and/or ZnO, the metal oxide mol ratio of doping be no more than the pressure
The 5% of Bi and Pb elements mole sum in electroceramics.
It is preferred that being also added with binding agent in the metal oxide powder, binding agent includes PVA, PVB, the bonding
Agent quality is the 5-10wt% of metal oxide powder.
It is preferred that by suppressing to obtain the pressure under 50-500MPa, to the compacting of material powder isostatic cool pressing or tablet press machine
Electroceramics biscuit.
It is preferred that sintering time is 1-20 hours in step 2), heating rate and rate of temperature fall are 0.5-6 DEG C/min.
It is preferred that being polarized in step 3) in silicone oil 20-40 minutes, poling temperature is 25-150 DEG C, polarizing voltage 3-
7KV/mm。
Beneficial effects of the present invention：
Titanium magnesium acid bismuth-lead titanate piezoelectric ceramics of prepared Tetragonal, with generally preparing positioned at accurate with phase boundary week
Enclose, i.e. (1-x) Bi (Mg1/2Ti1/2)O3-xPbTiO3(x≤0.42) is compared, and its temperature in use has increased significantly, from 400
Below DEG C, more than 600 DEG C are brought up to, improves 200 DEG C.For the preferred component of 0.55≤x≤0.70, its temperature in use is even
Reach 650 DEG C.The optimal sample of individual components is after annealing at a temperature of 800 DEG C, its d33Still there is 100pC/N or so.In addition, sample
The dielectric loss of product is smaller, and less than 3%, and temperature stability is good.Material involved in the present invention disclosure satisfy that many high temperature necks
Domain is simultaneously to the requirement in terms of piezoelectric performance and temperature in use and temperature stability.In addition, the method process equipment is simple,
Easy to operate, energy consumption is low, short preparation period, is easy to mass produce, is advantageously implemented industrial applications.
Brief description of the drawings
Fig. 1 shows the Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectric ceramics prepared in an embodiment of the invention
XRD spectrum.
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
The present invention is merely to illustrate, is not intended to limit the present invention.
The invention discloses a kind of Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectric ceramics suitable for high-temperature field, and it is changed
Formula is (1-x) Bi (Mg1/2Ti1/2)O3-xPbTiO3, wherein 0.50≤x≤0.90.
Preferably, 0.55≤x≤0.70.
More electedly, 0.58≤x≤0.64.
It can be mixed using manganese ion, chromium ion, copper ion, niobium ion, lanthanum ion, nickel ion and zinc ion etc.
It is miscellaneous.
It is preferred that manganese ion is doped.
Preparation method is：
Step A) ceramic powder preparation, prepared composition is (1-x) Bi (Mg first1/2Ti1/2)O3-xPbTiO3(wherein 0.50
≤ x≤0.90) powder；
Step B) make blank：The binding agents such as a certain amount of PVA, PVB, which are added, in the powder that step A is obtained passes through ball milling
It is blank (biscuit) in 50-500MPa forming under the pressure after machine is well mixed；
Step C) sintering：The powder of the upper identical component of blank covering after shaping, is inserted in the crucible put upside down,
Calcining 1-20 hours obtain block ceramic at a temperature of 1000-1150 DEG C；
Step D) by electrode and polarization：By obtained block is shaped and size after be covered with silver electrode or
Platinum electrode, polarized in silicone oil 20-40 minutes, poling temperature is 25-150 DEG C, polarizing voltage 3-7KV/mm.
Step A) in, also using MnO2、Cr2O3、CuO、Nb2O5、La2O3, NiO and/or ZnO etc. be to (1-x) Bi (Mg1/ 2Ti1/2)O3-xPbTiO3It is doped, doping is no more than (1-x) Bi (Mg1/2Ti1/2)O3-xPbTiO3The 5% of molar fraction.
Step A) in, solid phase reaction can be included by preparing the method for powder, collosol and gel, the methods of co-precipitation.
Step B) in, the amount of described binding agent is 5-10wt%, preferably 6%-7%.
Step B) in, described forming method can be the methods of isostatic cool pressing is suppressed or tablet press machine is suppressed.
Step C) in sintering heating rate and rate of temperature fall be 0.5-6 DEG C/min.
The present invention has carried out further expansion to the composition of titanium magnesium acid bismuth-lead titanates system piezoelectric ceramics, makes its composition
The accurate same phase boundary regions of larger deviation, into square area, obtain a kind of new Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectricity
Ceramics.It is with standard with phase boundary ambient components, i.e. (1-x) Bi (Mg1/2Ti1/2)O3-xPbTiO3The sample of (x≤0.42) is compared, and is made
Significantly raised with temperature, temperature in use is higher than 600 DEG C.For the preferred component of 0.55≤x≤0.70, its temperature in use is very
To reaching 650 DEG C.The optimal sample of individual components is after annealing at a temperature of 800 DEG C, its d33Still there is 100pC/N or so.In addition,
The dielectric loss of sample is smaller, and less than 3%, and temperature stability is good.With standard with (1-x) Bi (Mg near phase boundary1/2Ti1/2)
O3-xPbTiO3(x≤0.42) is compared, and Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectric ceramics can be under more extensive occasion
Using it is very huge and wide that this series of advantage make it that it has in ultrasonic transducer, driver and senser element etc.
General application prospect.In addition, the method process equipment is simple, easy to operate, energy consumption is low, short preparation period, is easy to extensive life
Production, is advantageously implemented industrial applications.
Some exemplary embodiments are included further below so that the present invention is better described.It should be understood that the present invention is in detail
The above-mentioned embodiment stated, and following examples are only illustrative of the invention and is not intended to limit the scope of the invention, this area
Technical staff the protection of the present invention is belonged to according to some nonessential modifications and adaptations for making of the above of the present invention
Scope.In addition, specific proportioning, time, temperature in following technological parameters etc. is also only exemplary, those skilled in the art can be with
Suitable value is selected in the range of above-mentioned restriction.
Embodiment 1
It is 0.50Bi (Mg by sol-gal process prepared composition1/2Ti1/2)O3-0.50PbTiO3Powder.Add in powder
Enter total quality of material be divided into 5wt% PVA by ball mill it is well mixed after, pass through in 50MPa pressure and cold wait pressurization to suppress
Into blank.The powder of one layer of identical component is covered on the blank suppressed, then a crucible on back-off, with 4 DEG C/h liter
Warm speed rises to 1050 DEG C and is incubated 20 hours, is then down to room temperature with 4 DEG C/h rate of temperature fall, obtains block body ceramic material.Will
Painting is covered with silver electrode after block materials are processed into certain shape and size, is being polarized 20 minutes in silicone oil, poling temperature is
150 DEG C, polarizing voltage 3KV/mm；
The type high-temperature dielectric temperature spectrum testing systems of GJW- I produced using electronic material research institute of Xi'an Communications University determine sample
The Curie temperature of product, the ZJ-3A type quasistatics d produced by Chinese Academy of Sciences's acoustics33The normal temperature pressure of measuring instrument test sample
Electric constant, the piezoelectric monocrystal prepared in embodiment 1 is tested, obtaining piezoelectric monocrystal Curie temperature made from embodiment 1 is
485-495 DEG C, piezoelectric constant 80-120pC/N, for sample after return of goods 2h at a temperature of 700 DEG C, its piezoelectric constant is still high in addition
In 100pC/N.
Embodiment 2
It is 0.45Bi (Mg by coprecipitation prepared composition1/2Ti1/2)O3-0.55PbTiO3Powder, added in powder
Total quality of material be divided into 10wt% PVB by ball mill it is well mixed after, be pressed into 300MPa pressure by tablet press machine
Blank.The powder of one layer of identical component is covered on the blank suppressed, then a crucible on back-off, with 3 DEG C/h heating
Speed rises to 1050 DEG C and is incubated 10 hours, is then down to room temperature with 3 DEG C/h rate of temperature fall, obtains block body ceramic material.By block
Painting is covered with silver electrode after body material is processed into certain shape and size, is being polarized 25 minutes in silicone oil, poling temperature 130
DEG C, polarizing voltage 4KV/mm；
After tested, piezoelectric monocrystal Curie temperature made from embodiment 2 is 497-500 DEG C, piezoelectric constant 75-110pC/N,
In addition for sample after return of goods 2h at a temperature of 750 DEG C, its piezoelectric constant remains above 90pC/N.
Embodiment 3
By high-purity MgO, TiO2、Bi2O3And Pb3O4Chemical formula 0.40Bi (Mg are pressed with PbO mixture1/2Ti1/2)O3-
0.60PbTiO3Stoichiometric proportion dispensing, add in addition total material molar fraction be 2% MnO2, mixed by ball mill equal
After even, powder is prepared using solid phase reaction.Total quality of material is added in powder and is divided into 6wt% PVA by ball mill again
After well mixed, blank is pressed into by tablet press machine in 500MPa pressure.On the blank suppressed cover one layer it is identical into
The powder divided, then a crucible on back-off, rises to 1100 DEG C with 0.5 DEG C/h heating rate and is incubated 10 hours, then with 0.5
DEG C/h rate of temperature fall is down to room temperature, obtain block body ceramic material.Applied after block materials to be processed into certain shape and size
Platinum electrode is covered with, is being polarized 30 minutes in silicone oil, poling temperature is 120 DEG C, polarizing voltage 5KV/mm；
After tested, piezoelectric monocrystal Curie temperature made from embodiment 3 is 500-510 DEG C, piezoelectric constant 75-100pC/N,
Electromechanical coupling factor is 42%-46%, dielectric loss 1%-3%, in addition sample after return of goods 2h at a temperature of 800 DEG C, its
Piezoelectric constant still reaches 85pC/N or so.
Embodiment 4
It is 0.38Bi (Mg by sol-gal process prepared composition1/2Ti1/2)O3-0.62PbTiO3Powder (its XRD such as Fig. 1
It is shown), added in powder total quality of material be divided into 7wt% PVA by ball mill it is well mixed after, in 200MPa pressure
Blank is pressed into by tablet press machine.The powder of one layer of identical component is covered on the blank suppressed, then an earthenware on back-off
Crucible, rise to 1150 DEG C with 2 DEG C/h heating rate and be incubated 2 hours, room temperature is then down to 2 DEG C/h rate of temperature fall, obtains block
Body ceramic material.Painting is covered with platinum electrode after block materials to be processed into certain shape and size, is being polarized 35 points in silicone oil
Clock, poling temperature are 80 DEG C, polarizing voltage 6KV/mm；
From Fig. 1, it can be seen that the titanium magnesium acid bismuth-lead titanate monocrystal to grow out is pure Tetragonal perovskite structure；
After tested, piezoelectric monocrystal Curie temperature made from embodiment 4 is 505-520 DEG C, piezoelectric constant 70-100pC/N,
Electromechanical coupling factor is 40%-45%, dielectric loss 1%-2.5%, in addition sample after return of goods 2h at a temperature of 800 DEG C,
Its piezoelectric constant still reaches 80pC/N.
Embodiment 5
By high-purity MgO, TiO2、Bi2O3And Pb3O4Chemical formula 0.20Bi (Mg are pressed with PbO mixture1/2Ti1/2)O3-
0.80PbTiO3Stoichiometric proportion dispensing, add in addition total material molar fraction be 2% Nb2O5, mixed in ball mill equal
It is even, obtain powder using solid phase reaction.Total quality of material is added in powder it is divided into 7wt% PVB and is mixed again by ball mill
After closing uniformly, blank is pressed into by isostatic cool pressing in 100MPa pressure.On the blank suppressed cover one layer it is identical into
The powder divided, then a crucible on back-off, rises to 1100 DEG C with 6 DEG C/h heating rate and is incubated 10 hours, then with 6 DEG C/h
Rate of temperature fall be down to room temperature, obtain block body ceramic material.Block materials are processed into after certain shape and size to apply and be covered with
Platinum electrode, polarized 40 minutes in silicone oil, poling temperature is 25 DEG C, polarizing voltage 7KV/mm.
Claims (9)
- A kind of 1. preparation method of Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectric ceramics, it is characterised in that the Tetragonal titanium magnesium The constitutional chemistry formula of sour bismuth-lead titanate piezoelectric ceramics is (1-x)Bi(Mg1/2Ti1/2)O3 -xPbTiO3, wherein 0.50≤x≦ 0.90, methods described includes：1）By the mol ratio between metallic element in the Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectric ceramics constitutional chemistry formula, Metal oxide powder is weighed, wherein, Bi oxide is Bi2O3, Mg oxide is MgO, and Ti oxide is TiO2, Pb Oxide be PbO and/or Pb3O4；2）First by step 1）Weigh progress forming processes after metal oxide powder uniformly mixes and obtain piezoelectric ceramics biscuit, then Piezoelectric ceramics biscuit is obtained into block ceramic in 1000-1200 DEG C of sintering；3）By step 2）The block ceramic of preparation is covered with silver electrode or platinum electrode, and polarization process is carried out in silicone oil.
- 2. preparation method according to claim 1, it is characterised in that 0.55≤x≦0.70。
- 3. preparation method according to claim 2, it is characterised in that 0.58≤x≦0.64。
- 4. preparation method according to claim 1, it is characterised in that also contain in the metal oxide powder and be used to mix The MnO of miscellaneous Tetragonal titanium magnesium acid bismuth-lead titanate piezoelectric ceramics2、Cr2O3、CuO、Nb2O5、La2O3, NiO and/or ZnO, doping Metal oxide mol ratio be no more than the piezoelectric ceramics in Bi and Pb element mole sums 5%.
- 5. preparation method according to claim 1, it is characterised in that also added with bonding in the metal oxide powder Agent, binding agent include PVA, PVB, and the binding agent quality is the 5-10wt% of metal oxide powder.
- 6. preparation method according to claim 1, it is characterised in that by being used under 50-500MPa, to material powder Tablet press machine is suppressed to obtain the piezoelectric ceramics biscuit.
- 7. preparation method according to claim 6, it is characterised in that the tablet press machine is compressed to isostatic cool pressing compacting.
- 8. preparation method according to claim 1, it is characterised in that step 2）The middle sintered heat insulating time is 1-20 hours, Heating rate and rate of temperature fall are 0.5-6 DEG C/min.
- 9. according to any described preparation method in claim 1-8, it is characterised in that step 3）In polarized in silicone oil 20- 40 minutes, poling temperature was 25-150 DEG C, and polarizing voltage is 3-7 KV/mm.
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| CN112159227B (en) * | 2020-10-11 | 2023-04-04 | 浙江清华长三角研究院 | Potassium-sodium niobate-based leadless piezoelectric ceramic and manufacturing process thereof |
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| CN116375466A (en) * | 2023-04-04 | 2023-07-04 | 湖南瀚德微创医疗科技有限公司 | Piezoelectric ceramic and preparation method thereof |
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