CN104150898A - Leadless piezoelectric ceramic material capable of being sintered at low temperature and preparation method of leadless piezoelectric ceramic material - Google Patents
Leadless piezoelectric ceramic material capable of being sintered at low temperature and preparation method of leadless piezoelectric ceramic material Download PDFInfo
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Abstract
The invention discloses a leadless piezoelectric ceramic material capable of being sintered at a low temperature. The leadless piezoelectric ceramic material is composed of [Bi(1.002-X)Na(1.002-5X)K4X]0.5TiO3-(X-0.002)BaTiO3+Y%Li2CO3+M%Fe2O3+W%ZnO, wherein X is not smaller than 0.025 and is not greater than 0.035; Y is greater than 0 and is not greater than 2; M is greater than 0 and is not greater than 3; W is greater than 0 and is not greater than 0.2. A preparation method of the leadless piezoelectric ceramic material comprises the following steps: weighing raw materials, performing wet ball milling on the raw materials to uniformly mix the raw materials, and then drying, pre-sintering, crushing and sieving the raw materials; adding Y%Li2CO3, M%Fe2O3 and W%ZnO, and performing fine grinding, binder addition for granulation, molding, binder removal, sintering and polarization. The leadless piezoelectric ceramic material is low in sintering temperature and lead-free, and can be quickly produced on a large scale; a larger piezoelectric coefficient, a larger electromechanical coupling coefficient, a high Curie point and a high dielectric constant are obtained; requirements of a low-temperature co-sintering ceramic piezoelectric device with a lamination type structure are met.
Description
Technical field
The present invention relates to a kind of low temperature sintering lead-free piezoceramic material and preparation method thereof, a kind of low temperature sintering many oxide doping bismuthino uhligite lead-free piezoceramic material and preparation method thereof particularly, belongs to the technical field of lead-free piezoceramic material.
Background technology
Piezoelectric ceramics can adaptive environment variation realize the mutual conversion between mechanical energy and electric energy, there is collection sensing, carry out and be controlled in the particular attribute of one, be a kind of important functional materials.Piezoelectric ceramics is with its unique performance, and the application in the fields such as business, military affairs, automobile, computer, medical science, machinery, electronics, communication and consumption is increasingly extensive, spreads all over the every nook and cranny in people's daily life.Traditional piezoelectric ceramics is to take the leaded pottery of polynary system that PZT is base, but one of main component of PZT base pottery is volatile toxic substance PbO, the content of its PbO, all more than 50%, causes very large harm to environment and human body in sintering process and after discarded.Meanwhile, due to the boiling characteristics of PbO, homogeneity of product and repeatability are reduced.In the preparation and fabrication of many conventional piezoelectric stupaliths, not only a large amount of consumption of natural resource and the energy, and can cause serious ecological environmental pollution.
In recent years, along with the demand of environment protection and human social, research and development novel environmental close friend's piezoelectric ceramics has become developed country and has endeavoured one of focus material of research and development.Calendar year 2001, European Parliament passed through the decree about " limiting objectionable impurities in electron device and electronics ", and implemented due to 2008.Wherein in being limited the material using, just comprise plumbous piezoelectric device.1,510,000 Euros of research and development of carrying out about leadless piezoelectric ceramics of European Economic Community's project verification for this reason.The U.S. and Japan and China Ministry of Industry and Information have also passed through similar decree in succession, and improve year by year the supporting dynamics to development leadless piezoelectric ceramics project.Therefore, development is a urgent challenge and is significant without the existing leaded piezoceramic material of environment compatibility piezoelectric ceramics replacement of lead base.
Current lead-free piezoceramic material mainly contains BaTiO
3base, Bi
1/2na
1/2tiO
3(BNT) base, niobate, bismuthino laminated leadless piezoelectric ceramic etc.Na wherein
0.5k
0.5nbO
3(KNN) piezoceramic material belongs to perovskite structure, and its Curie temperature is about 415 ℃, is oblique side's phase under room temperature, is regarded as substituting one of candidate material of conventional P ZT piezoelectric ceramics.But these novel lead-free piezoceramic material sintering temperatures are higher, reach 1200 ~ 1300 ℃, caused the waste of the energy and resource.In order to save the energy, reduce carbon emission amount, exploring a kind of low temperature sintering lead-free piezoceramic material becomes the Key technique problem that current urgent need solves.
The invention discloses a kind of low temperature sintering many oxide doping bismuthino uhligite lead-free piezoceramic material and preparation method thereof, matrix stupalith consists of [Bi
(1.002-X)na
(1.002-5X)k
4X]
0.5tiO
3(X-0.002) BaTiO
3.This system has high tension electricity coefficient, high electromechanical coupling factor and high-curie temperature, is the critical material of electromechanical transducer and piezoelectric actuator.Conventionally this system piezoelectric ceramics sintering temperature is higher, and at 1100 ~ 1200 ℃, the present invention adulterates to reduce the sintering temperature of piezoceramic material by many oxide, keeps good piezoelectric property, electromechanical coupling performance and dielectric properties simultaneously.Can be widely used in the fields such as business, military affairs, automobile, computer, medical science, machinery, electronics, communication and consumption, meet the requirement of lamination sheet type Structures at Low Temperature common burning porcelain piezoelectric device.
Summary of the invention
The invention provides a kind of low temperature sintering many oxide doping bismuthino uhligite lead-free piezoceramic material and preparation method thereof, object is that the existing piezoelectric ceramics sintering temperature of solution is high, causes the problems such as environmental pollution.Product of the present invention has good piezoelectric property and dielectric properties, high electromechanical coupling factor and high-curie temperature, and preparation method's good economy performance, technique are simple, power consumption less, pollution-free etc.
Technical problem to be solved by this invention is achieved through the following technical solutions.
A low temperature sintering lead-free piezoceramic material, its chemical general formula is,
[Bi
(1.002-X)Na
(1.002-5X)K
4X]
0.5TiO
3 -(X-0.002)BaTiO
3＋Y%Li
2CO
3＋M%Fe
2O
3＋W%ZnO
Wherein, [Bi
(1.002-X)na
(1.002-5X)k
4X]
0.5tiO
3-(X-0.002) BaTiO
3for matrix stupalith, Y% represents Li
2cO
3account for the weight percent of matrix stupalith; M% represents Fe
2o
3account for the weight percent of matrix stupalith; W% represents that ZnO accounts for the weight percent of matrix stupalith.
On the basis of technique scheme, 0.025≤X≤0.035 in described composition, 0 < Y≤2,0 < M≤3,0 < W≤0.2.
On the basis of technique scheme, the present invention also provides a kind of manufacture method of low temperature sintering lead-free piezoceramic material, and it comprises the following steps:
A) by Bi
2o
3, Na
2cO
3, K
2cO
3, BaCO
3, TiO
2material powder is by [Bi
(1.002-X)na
(1.002-5X)k
4X]
0.5tiO
3(X-0.002) BaTiO
3stoichiometric ratio prepare burden, wet ball grinding mixes it, then dries;
B) step a gained powder is placed in crucible and carries out pre-burning,, at 850 ~ 900 ℃ of insulation 2 ~ 3h, then pulverize, sieve;
C) take Y%Li
2cO
3, M%Fe
2o
3add in step b gained powder and carry out fine grinding with W%ZnO, 0 < Y≤2 wherein, 0 < M≤3,0 < W≤0.2;
D) after step c ball milling certain hour, adding 3 ~ 5wt% concentration is the high polymer binder of 10 ~ 15wt%, then ball milling 1 ~ 2 hour, mixes granulation, moulding, binder removal, sintering;
E) stupalith of steps d gained is carried out to cold working, ultrasonic cleaning, by silver, polarization.Silver, the comma in the middle of polarization does not know to want.
On the basis of technique scheme, wet ball grinding in described step a adopts dehydrated alcohol to make solvent, and zirconia ball is done ball-milling medium, and described zirconia ball: dehydrated alcohol is that weight ratio is the ratio mixing of 1:1.8 ~ 2:0.6 ~ 0.8, ball milling 6 ~ 8 hours, then 60 ~ 80 ℃ of oven dry.
On the basis of technique scheme, fine grinding in described step c is wet ball grinding, adopts deionized water to make solvent, and zirconia ball is done ball-milling medium, according to material: zirconia ball: deionized water is that the ratio of weight ratio 1:1.8 ~ 2:0.8 ~ 1 is mixed, ball milling 8 ~ 10 hours.
The high polymer binder that described steps d is added is the aqueous solution of polyvinyl alcohol, and concentration is 10 ~ 15wt%.
On the basis of technique scheme, the forming pressure of described steps d is 16 ~ 17MPa.
On the basis of technique scheme, the dump temperature of described steps d is 450 ~ 550 ℃ of insulations 1 ~ 2 hour.
On the basis of technique scheme, the sintering temperature of described steps d is 880 ~ 950 ℃ of insulations 2 ~ 3 hours.
On the basis of technique scheme, the polarization in described step e is to process 10 ~ 30min under 60 ~ 80 ℃, 3 ~ 4Kv/mm.
Compared with prior art, advantage of the present invention is as follows:
1. low temperature sintering many oxide of the present invention doping bismuthino uhligite lead-free piezoceramic material, it is a kind of bismuthino perovskite typed piezoceramic material, it is the critical material of electromechanical transducer and piezoelectric actuator, the doping of employing many oxide, effectively reduces sintering temperature (<950 ℃).
2. high (the d of low temperature sintering many oxide of the present invention doping bismuthino uhligite lead-free piezoceramic material piezo-electric modulus
33=245 ~ 265 pc/N), the high (k of electromechanical coupling factor
p=24 ~ 28%), Curie temperature high (>285 ℃), the high (ε of specific inductivity
r=750 ~ 1165), dielectric loss little (tan δ <5%), meets the application requiring of monolithic multilayer structure LTCC piezoelectric device to stupalith.
3. preparation method's technique of the present invention is simple, adopts conventional production unit, and with short production cycle, production cost is low.
4. energy-conservation, the material-saving of the preparation method of this piezoceramic material, green, environmental protection, meet the RoHS of European Union instruction, not leaded Pb, cadmium Cd, mercury Hg, sexavalent chrome Cr
6+, the objectionable impurities such as Polybrominated biphenyl PBBs, Poly Brominated Diphenyl Ethers PBDEs, reduced to the full extent the environmental pollution bringing in raw material, waste material and production process.
Embodiment
The present invention further illustrates by the following examples.
embodiment 1
By chemical constitution [Bi
0.977na
0.877k
0.1]
0.5tiO
30.023BaTiO
3+ 0.5%Li
2cO
3+ 1%Fe
2o
3+ 0.2%ZnO, calculates various raw material Bi
2o
3, Na
2cO
3, K
2cO
3, BaCO
3, TiO
2proportioning, weighs with electronic analytical balance, puts into ball grinder, adopt dehydrated alcohol to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: dehydrated alcohol is that the ratio of weight ratio 1:2:0.6 is mixed, wet ball grinding 6 hours, then 80 ℃ of oven dry.The lumpy material obtaining is placed on to 850 ℃ of pre-burnings, insulation 3h, then pulverize and sieve.According to Li
2cO
3, Fe
2o
3, the ZnO per-cent that accounts for ceramic matrix weighs and to add in ceramic base-material, adopts deionized water to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: deionized water is that the ratio of weight ratio 1:2:0.6 is mixed, wet ball grinding 8h.Add the 3%PVA aqueous solution (concentration 15%wt), ball milling 2h, mixes rear taking-up granulation, at 17MPa forming under the pressure.With 2 ℃/min temperature rise rate to 500 ℃ binder removal 1h, with 3 ℃/min, be raised to 890 ℃ of sintering 2h.The sample obtaining passes through polishing again, by silver, at 70 ℃, the 4Kv/mm 10min that polarizes.Through test, its test result is as follows: piezoelectric coefficient d
33=250pc/N, electromechanical coupling factor k
p=26.8%, Curie temperature T
c=298 ℃, DIELECTRIC CONSTANT ε
r=750, dielectric loss tan δ <4.5%.
embodiment 2
By chemical constitution [Bi
0.972na
0.852k
0.12]
0.5tiO
30.028BaTiO
3+ 2%Li
2cO
3+ 1.5%Fe
2o
3+ 0.2%ZnO, calculates various raw material Bi
2o
3, Na
2cO
3, K
2cO
3, BaCO
3, TiO
2proportioning, weighs with electronic analytical balance, puts into ball grinder, adopt dehydrated alcohol to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: dehydrated alcohol is that the ratio of weight ratio 1:1.8:0.8 is mixed, wet ball grinding 7 hours, then 70 ℃ of oven dry.The lumpy material obtaining is placed on to 870 ℃ of pre-burnings, insulation 3h, then pulverize and sieve.According to Li
2cO
3, Fe
2o
3, the ZnO per-cent that accounts for ceramic matrix weighs and to add in ceramic base-material, adopts deionized water to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: deionized water is that the ratio of weight ratio 1:1.8:0.8 is mixed, wet ball grinding 8h.Add the 4%PVA aqueous solution (concentration 12%wt), ball milling 2h, mixes rear taking-up granulation, at 16MPa forming under the pressure.With 2 ℃/min temperature rise rate to 450 ℃ binder removal 2h, with 3 ℃/min, be raised to 920 ℃ of sintering 3h.The sample obtaining passes through polishing again, by silver, at 80 ℃, the 4Kv/mm 10min that polarizes.Through test, its test result is as follows: piezoelectric coefficient d
33=265 pc/N, electromechanical coupling factor k
p=25.9%, Curie temperature T
c=290 ℃, DIELECTRIC CONSTANT ε
r=1080, dielectric loss tan δ <3.9%.
embodiment 3
By chemical constitution [Bi
0.967na
0.827k
0.14]
0.5tiO
30.033BaTiO
3+ 1%Li
2cO
3+ 2.5%Fe
2o
3+ 0.1%ZnO, calculates various raw material Bi
2o
3, Na
2cO
3, K
2cO
3, BaCO
3, TiO
2proportioning, weighs with electronic analytical balance, puts into ball grinder, adopt dehydrated alcohol to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: dehydrated alcohol is that the ratio of weight ratio 1:1.9:0.7 is mixed, wet ball grinding 8 hours, then 80 ℃ of oven dry.The lumpy material obtaining is placed on to 880 ℃ of pre-burnings, insulation 2h, then pulverize and sieve.According to Li
2cO
3, Fe
2o
3, the ZnO per-cent that accounts for ceramic matrix weighs and to add in ceramic base-material, adopts deionized water to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: deionized water is that the ratio of weight ratio 1:2:0.8 is mixed, wet ball grinding 6h.Add the 4%PVA aqueous solution (concentration 12%wt), ball milling 1.5h, mixes rear taking-up granulation, at 17MPa forming under the pressure.With 2 ℃/min temperature rise rate to 500 ℃ binder removal 2h, with 3 ℃/min, be raised to 880 ℃ of sintering 3h.The sample obtaining passes through polishing again, by silver, at 60 ℃, the 3Kv/mm 30min that polarizes.Through test, its test result is as follows: piezoelectric coefficient d
33=248 pc/N, electromechanical coupling factor k
p=24.2%, Curie temperature T
c=280 ℃, DIELECTRIC CONSTANT ε
r=850, dielectric loss tan δ <4.3%.
embodiment 4
By chemical constitution [Bi
0.974na
0.862k
0.112]
0.5tiO
30.026BaTiO
3+ 1.5%Li
2cO
3+ 3%Fe
2o
3+ 0.2%ZnO, calculates various raw material Bi
2o
3, Na
2cO
3, K
2cO
3, BaCO
3, TiO
2proportioning, weighs with electronic analytical balance, puts into ball grinder, adopt dehydrated alcohol to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: dehydrated alcohol is that the ratio of weight ratio 1:1.8:0.6 is mixed, wet ball grinding 8 hours, then 60 ℃ of oven dry.The lumpy material obtaining is placed on to 890 ℃ of pre-burnings, insulation 3h, then pulverize and sieve.According to Li
2cO
3, Fe
2o
3, the ZnO per-cent that accounts for ceramic matrix weighs and to add in ceramic base-material, adopts deionized water to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: deionized water is that the ratio of weight ratio 1:1.9:0.7 is mixed, wet ball grinding 7h.Add the 5%PVA aqueous solution (concentration 10%wt), ball milling 1.5h, mixes rear taking-up granulation, at 16MPa forming under the pressure.With 2 ℃/min temperature rise rate to 550 ℃ binder removal 1h, with 3 ℃/min, be raised to 945 ℃ of sintering 2h.The sample obtaining passes through polishing again, by silver, at 80 ℃, the 4Kv/mm 20min that polarizes.Through test, its test result is as follows: piezoelectric coefficient d
33=245 pc/N, electromechanical coupling factor k
p=28.2%, Curie temperature T
c=304 ℃, DIELECTRIC CONSTANT ε
r=1165, dielectric loss tan δ <4.1%.
embodiment 5
By chemical constitution [Bi
0.97na
0.842k
0.128]
0.5tiO
30.03BaTiO
3+ 2%Li
2cO
3+ 2%Fe
2o
3+ 0.1%ZnO, calculates various raw material Bi
2o
3, Na
2cO
3, K
2cO
3, BaCO
3, TiO
2proportioning, weighs with electronic analytical balance, puts into ball grinder, adopt dehydrated alcohol to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: dehydrated alcohol is that the ratio of weight ratio 1:2:0.8 is mixed, wet ball grinding 8 hours, then 70 ℃ of oven dry.The lumpy material obtaining is placed on to 900 ℃ of pre-burnings, insulation 2h, then pulverize and sieve.According to Li
2cO
3, Fe
2o
3, the ZnO per-cent that accounts for ceramic matrix weighs and to add in ceramic base-material, adopts deionized water to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: deionized water is that the ratio of weight ratio 1:1.8:0.8 is mixed, wet ball grinding 6h.Add the 3%PVA aqueous solution (concentration 15%wt), ball milling 1h, mixes rear taking-up granulation, at 17MPa forming under the pressure.With 2 ℃/min temperature rise rate to 500 ℃ binder removal 1h, with 3 ℃/min, be raised to 930 ℃ of sintering 3h.The sample obtaining passes through polishing again, by silver, at 70 ℃, the 4Kv/mm 15min that polarizes.Through test, its test result is as follows: piezoelectric coefficient d
33=250 pc/N, electromechanical coupling factor k
p=25.3%, Curie temperature T
c=296 ℃, DIELECTRIC CONSTANT ε
r=960, dielectric loss tan δ <4.3%.
Performance test methods and the equipment of the low temperature sintering many oxide doping bismuthino uhligite lead-free piezoceramic material that in embodiments of the present invention, prepared by employing aforesaid method are as follows:
(1) piezo-electric modulus test
Piezoelectric coefficient d
33test according to the method for the test > >-5.5 cylinder longitudinal length extension vibration modes regulation of GB/T 3389-2008 < < piezoceramic material performance test methods performance perameter, carry out.
(2) electromechanical coupling factor k
p
Electromechanical coupling factor k
ptest according to the method for GB GB/T 2414.1-1998 < < piezoceramic material performance test methods disk radial extension vibration mode > > regulation, carry out.
(3) Curie temperature Tc
The test of Curie temperature Tc is carried out according to the method for the test > >-5.1 Curie temperature regulation of GB GB/T 3389-2008 < < piezoceramic material performance test methods performance perameter.
(4) dielectric properties test
By completing, by silver-colored ceramics sample, be placed on that on TH2613A type capacitance measuring tester, to test test frequency under room temperature environment be capacitance and the dielectric loss under 1KHz.Then according to the relative permittivity ε of formula 1-1 Calculating material
r:
（1－1）
In this formula, the capacitance that C is material (F), A is sample upper and lower surface area (m
2), the thickness that t is sample (m), d is the diameter (m) of sample upper and lower surface, ε
0for permittivity of vacuum, ε
0=8.85 * 10
-12(F/m)
Table 1 embodiment of the present invention products obtained therefrom performance comparison
| Embodiment | Piezo-electric modulus | Electromechanical coupling factor | Curie temperature | Specific inductivity | Dielectric loss |
| 1 | 250pc/N | 26.8% | 298℃ | 750 | <4.5% |
| 2 | 265pc/N | 25.9% | 290℃ | 1080 | <3.9% |
| 3 | 248pc/N | 24.2% | 280℃ | 850 | <4.3% |
| 4 | 245pc/N | 28.2% | 304℃ | 1165 | <4.1% |
| 5 | 250pc/N | 25.3% | 285℃ | 960 | <4.3% |
The present invention forms and uses the method for many oxide doping by adjusting matrix formulation, improve its piezoelectricity over-all properties when reducing stupalith sintering temperature.Add appropriate low melting point sintering aid Li
2cO
3, Fe
2o
3, ZnO can be down to 950 ℃ even lower from 1100 ℃ by ceramic sintering temperature, and in the sintering later stage, enter lattice, the electric property of regulation and control piezoelectric ceramics; And add positive trivalent metal oxide as " soft " doping agent, and by valence state and vacant regulation and control, compensate, can make up because of deteriorated to stupalith piezoelectric property of sintering aid.Low temperature sintering many oxide doping bismuthino uhligite lead-free piezoceramic material provided by the invention meets the application requiring of monolithic multilayer structure LTCC piezoelectric device to stupalith.
Claims (10)
1.
onekind of low temperature sintering lead-free piezoceramic material, is characterized in that: its chemical general formula is,
[Bi
(1.002-X)Na
(1.002-5X)K
4X]
0.5TiO
3 -(X-0.002)BaTiO
3＋Y%Li
2CO
3＋M%Fe
2O
3＋W%ZnO
Wherein, [Bi
(1.002-X)na
(1.002-5X)k
4X]
0.5tiO
3-(X-0.002) BaTiO
3for matrix stupalith, Y% represents Li
2cO
3account for the weight percent of matrix stupalith; M% represents Fe
2o
3account for the weight percent of matrix stupalith; W% represents that ZnO accounts for the weight percent of matrix stupalith.
2. a kind of low temperature sintering lead-free piezoceramic material according to claim 1, it is characterized in that: 0.025≤X≤0.035 in described composition, 0 < Y≤2,0 < M≤3,0 < W≤0.2.
3. manufacture, according to a method for a kind of low temperature sintering lead-free piezoceramic material described in claim 1 or 2 any one, is characterized in that comprising the following steps:
A) by Bi
2o
3, Na
2cO
3, K
2cO
3, BaCO
3, TiO
2material powder is by [Bi
(1.002-X)na
(1.002-5X)k
4X]
0.5tiO
3(X-0.002) BaTiO
3stoichiometric ratio prepare burden, wet ball grinding mixes it, then dries;
B) step a gained powder is placed in crucible and carries out pre-burning,, at 850 ~ 900 ℃ of insulation 2 ~ 3h, then pulverize, sieve;
C) take Y%Li
2cO
3, M%Fe
2o
3add in step b gained powder and carry out fine grinding with W%ZnO, 0 < Y≤2 wherein, 0 < M≤3,0 < W≤0.2;
D) after step c ball milling certain hour, adding 3 ~ 5wt% concentration is the high polymer binder of 10 ~ 15wt%, then ball milling 1 ~ 2 hour, mixes granulation, moulding, binder removal, sintering;
E) stupalith of steps d gained is carried out to cold working, ultrasonic cleaning, by silver, polarization.
4. the method for a kind of low temperature sintering lead-free piezoceramic material according to claim 3, it is characterized in that: the wet ball grinding in described step a adopts dehydrated alcohol to make solvent, zirconia ball is done ball-milling medium, and described zirconia ball: dehydrated alcohol is that the ratio of weight ratio 1:1.8 ~ 2:0.6 ~ 0.8 is mixed, ball milling 6 ~ 8 hours, then 60 ~ 80 ℃ of oven dry.
5. the method for a kind of low temperature sintering lead-free piezoceramic material according to claim 3, it is characterized in that: the fine grinding in described step c is wet ball grinding, adopt deionized water to make solvent, zirconia ball is done ball-milling medium, according to material: zirconia ball: deionized water is that the ratio of weight ratio 1:1.8 ~ 2:0.8 ~ 1 is mixed, ball milling 8 ~ 10 hours.
6. the method for a kind of low temperature sintering lead-free piezoceramic material according to claim 3, is characterized in that: the aqueous solution that the high polymer binder that described steps d is added is polyvinyl alcohol, concentration is 10 ~ 15wt%.
7. the method for a kind of low temperature sintering lead-free piezoceramic material according to claim 3, is characterized in that: the forming pressure of described steps d is 16 ~ 17MPa.
8. the method for a kind of low temperature sintering lead-free piezoceramic material according to claim 3, is characterized in that: the dump temperature of described steps d is 450 ~ 550 ℃ of insulations 1 ~ 2 hour.
9. the method for a kind of low temperature sintering lead-free piezoceramic material according to claim 3, is characterized in that: the sintering temperature of described steps d is 880 ~ 950 ℃ of insulations 2 ~ 3 hours.
10. the method for a kind of low temperature sintering lead-free piezoceramic material according to claim 3, is characterized in that: the polarization in described step e is to process 10 ~ 30min under 60 ~ 80 ℃, 3 ~ 4Kv/mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106518121A (en) * | 2016-11-10 | 2017-03-22 | 佛山蓝途科技有限公司 | High-Curie-temperature leadless piezoelectric ceramic and preparation method thereof |
| CN109400146A (en) * | 2018-12-14 | 2019-03-01 | 中国人民解放军国防科技大学 | High Curie temperature piezoelectric ceramic and preparation method thereof |
| CN116102345A (en) * | 2023-01-04 | 2023-05-12 | 湖北大学 | Bismuth layered piezoelectric ceramic material and preparation method thereof |
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| CN103482973A (en) * | 2013-09-10 | 2014-01-01 | 天津大学 | Lead-free quaternary system electro-strain piezoelectric ceramic material, preparation method and product |
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| CN1673178A (en) * | 2005-01-04 | 2005-09-28 | 西北工业大学 | Bismuth sodium titanate-barium titanate base piezoelectric ceramic and its prepn process |
| CN102850050A (en) * | 2012-08-31 | 2013-01-02 | 华中科技大学 | Low temperature sintering piezoelectric ceramic material and preparation method thereof |
| CN103482973A (en) * | 2013-09-10 | 2014-01-01 | 天津大学 | Lead-free quaternary system electro-strain piezoelectric ceramic material, preparation method and product |
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| CN106518121A (en) * | 2016-11-10 | 2017-03-22 | 佛山蓝途科技有限公司 | High-Curie-temperature leadless piezoelectric ceramic and preparation method thereof |
| CN109400146A (en) * | 2018-12-14 | 2019-03-01 | 中国人民解放军国防科技大学 | High Curie temperature piezoelectric ceramic and preparation method thereof |
| CN109400146B (en) * | 2018-12-14 | 2021-06-18 | 中国人民解放军国防科技大学 | High Curie temperature piezoelectric ceramic and preparation method thereof |
| CN116102345A (en) * | 2023-01-04 | 2023-05-12 | 湖北大学 | Bismuth layered piezoelectric ceramic material and preparation method thereof |
| CN116102345B (en) * | 2023-01-04 | 2024-03-19 | 湖北大学 | Bismuth layered piezoelectric ceramic material and preparation method thereof |
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Application publication date: 20141119 |