CN1810714A - No-prebaking sodium bismuth titanate-barium titanate lead-less piezoelectric ceramic doping material and its prepn - Google Patents
No-prebaking sodium bismuth titanate-barium titanate lead-less piezoelectric ceramic doping material and its prepn Download PDFInfo
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- CN1810714A CN1810714A CN 200610018252 CN200610018252A CN1810714A CN 1810714 A CN1810714 A CN 1810714A CN 200610018252 CN200610018252 CN 200610018252 CN 200610018252 A CN200610018252 A CN 200610018252A CN 1810714 A CN1810714 A CN 1810714A
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- piezoelectric ceramic
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- barium titanate
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Abstract
The no-prebaking sodium bismuth titanate-barium tiatnate lead-less piezoelectric ceramic doping material has the composition expression of (1-x)Bi0.5Na0.5TiO3+xBaTiO3+yIn2O3, where, x is 0.06-0.08 wt% and y is 0-0.02 wt%. Compared with conventional process, the preparation process of the present invention has no pre-synthesis and fine grinding steps, saving in power consumption and production period, high efficiency and low cost, and the product has ferroelectric performance of d33 up to 190 and g33 up to 20, approaching that of lead-base piezoelectric ceramic.
Description
Technical field
The present invention relates to bismuth-sodium titanate---barium titanate lead-less piezoelectric ceramic, particularly do not have the pre-burning bismuth-sodium titanate---barium titanate lead-less piezoelectric ceramic dopant material and preparation method thereof.Belong to environment compatibility piezoceramic material field.
Background technology
As the important informational function stupalith of a class, piezoelectric ceramics has widely in the detection of various information, transmission, stores processor to be used.At present, the piezoelectric ceramics overwhelming majority who uses in the industrial production is with Pb-based lanthanumdoped zirconate titanates (Pb (Zr, Ti) O
3) or lead titanate (PbTiO
3) be the lead base piezoelectric ceramic composition of main component.This class piezoelectric ceramics material section has good piezoelectricity ferro performance, high Curie temperature.But, because Pb0 or Pb
3O
4At high temperature volatile, thus cause all can bringing serious harm in the treating processes of plumbous series piezoelectric ceramic after producing, use and discarding to human health and ecotope.
At present, people develop multiple leadless piezoelectric ceramics, wherein bismuth-sodium titanate---and the barium titanate lead-less piezoelectric ceramic effect is best.Its composition formula is (1-x) Bi
0.5Na
0.5TiO
3-xBaTiO
3, see that it is (1-x) Bi that document 1 (Journal of Inorganic Materials, Vol 15, No5,2000,12) has provided composition formula
0.5Na
0.5TiO
3-xBaTiO
3The leadless piezoelectric ceramics system, d
33=125pC/N, Kp=29%; It is (1-x) Bi that document 2 (TERIALS LETTERS, 58 (2004) 1194-1198) has provided composition formula
0.5Na
0.5TiO
3-xBaTiO
3The piezoelectric ceramic composition d of-Co
33=139pC/N, ε
T 33/ ε
0=1200; Document 3 (Harbin University of Science and Technology's journal, 2002,7 (6), 96-98) having provided composition formula is (1-x) Bi
0.5Na
0.5TiO
3-xBaTiO
3The piezoelectric ceramic composition of-Sb, d
33=172pC/N, ε
T 33/ ε
0=1540; It is Bi that Chinese invention patent prospectus CN1623954A provides composition formula
0.5Na
0.5TiO
3-xBa (Ti
1-yZr
y) O
3Piezoelectric ceramic composition, d
33=147pC/N, ε
T 33/ ε
0=881.4.But the above employing all is traditional sintering method, promptly earlier about 800 ℃ pre-synthetic after sintering again, the used like this energy and time are more, cost is higher in process of production to make it.
Summary of the invention
Purpose of the present invention is exactly for save energy, raises the efficiency, and reduces cost, and has proposed a kind of no pre-burning bismuth-sodium titanate---barium titanate lead-less piezoelectric ceramic dopant material and preparation method thereof.
The present invention is achieved in that its composition formula is (1-x) Bi
0.5Na
0.5TiO
3+ xBaTiO
3+ yIn
2O
3, 0.06≤x≤0.08,0≤y≤0.02wt% (wt is weight percentage) wherein.
Prepare leadless piezoelectric ceramics of the present invention and can adopt technical pure or chemical pure Bi
2O
3, Na
2CO
3, BaCO
3, TiO
2, In
2O
3Be raw material.
Have the preparation method of presintering preparation process as follows routinely:
1, general formula (1-x) Bi
0.5Na
0.5TiO
3+ xBaTiO
3+ yIn
2O
3The stoichiometric ratio raw materials weighing.
2, batching and alcohol are by 2g: 1ml puts into nylon ball grinder, and dress agate ball in jar ball milling 4-5 hour, makes batching thorough mixing and levigate.
3, will prepare burden to take out in the ball grinder and put baking oven, 100 ℃ of oven dry into.
4, the crucible of packing into of the batching after will drying is raised to 860 ℃ with 200 ℃/hour heat-up rate and is incubated 1-3 hour pre-burning again.
5, the batching of the bulk after the pre-burning is placed on nylon ball grinder, dress agate ball in jar, ball milling 4-5 hour.
6, will prepare burden to take out in the ball grinder and put baking oven, 100 ℃ of oven dry into.
7, the powder after will drying adds tackiness agent PVA, and thorough mixing is even, is 12mm in being pressed into diameter, and thickness is the disk of 1.3mm.
8, with the disk that presses 550 ℃ of following binder removals 2 hours.
9, treat the disk cool to room temperature after, the re-adjustment temperature rise rate was at 1100-1200 ℃ of following sintering 1-3 hour: in the temperature-fall period the 900-950 ℃ of insulation of annealing.
10, with silver electrode on the ceramic plate behind the sintering, in 20-100 ℃ silicone oil, with voltage polarizing 5-20 minute of 3-6kV/mm.
The preparation method of direct sintering of the present invention is as follows:
1, presses general formula (1-x) Bi
0.5Na
0.5TiO
3+ xBaTiO
2+ yIn
2O
3The stoichiometric ratio raw materials weighing.
2, will prepare burden and alcohol by 2g: 1ml puts into nylon ball grinder, and dress agate ball in jar ball milling 4-5 hour, makes batching thorough mixing and levigate.
3, put batching into baking oven, 100 ℃ of oven dry.
4, the powder after will drying adds tackiness agent PVA, and thorough mixing is even, and it is 12mm that dry-pressing becomes diameter, and thickness is the disk of 1.3mm.
5, with the disk that presses 550 ℃ of following binder removals 2 hours.
6, treat the disk cool to room temperature after, be warmed up to 800--850 ℃ by 200/ hour again, be incubated 2-3 hour, be warmed up to 1100--1200 ℃ by 150/ hour again, be incubated 1-3 hour; In the temperature-fall period the 900-950 ℃ of insulation of annealing.
7, with silver electrode on the ceramic plate behind the sintering, in 20-100 ℃ silicone oil, with voltage polarizing 5-20 minute of 3-6kV/mm.
The piezoelectric ceramics of this method preparation has good piezoelectricity ferro performance, d
33Reach more than 190 g
33Reach more than 20, approach the lead base performance of piezoelectric ceramics, and owing to removed the pre-synthetic step that reaches pre-synthetic back fine grinding, thereby saved a large amount of energy and production time, have practical value.
Embodiment
The present invention is further described with embodiment below.
Embodiment one
Prescription: 0.93Bi
0.5Na
0.5TiO
3+ 0.07BaTiO
3
Method: direct sintering
Performance: d
33(pC/N) g
33(x10
-3) tg θ (%) ε
T 33/ ε
0k
t/ k
p
166 19.98 3.35 939 1.49
Method: sintering again after 860 ℃ of following pre-burnings
Performance: d
33(pC/N) g
33(x10
-3) tg θ (%) ε
T 33/ ε
0k
t/ k
p
138 17.46 3.7 893 1.32
Embodiment two
Prescription: 0.93Bi
0.5Na
0.5TiO
3+ 0.07BaTiO
3+ 0.01wt%In
2O
3
Method: direct sintering
Performance: d
33(pC/N) g
33(x10
-3) tg θ (%) ε
T 33/ ε
0k
t/ k
p
183 20.3 43.43 1014 2.32
Method: sintering again after 880 ℃ of following pre-burnings
Performance: d
33(pC/N) g
33(x10
-3) tg θ (%) ε
T 33/ ε
0k
t/ k
p
138 20.12 3.80 775 1.58
Embodiment three
Prescription: 0.93Bi
0.5Na
0.5TiO
3+ 0.0TBaTiO
3+ 0.014wt%In
2O
3
Method: direct sintering
Performance: d
33(pC/N) g
33(x10
-3) tg θ (%) ε
T 33/ ε
0k
t/ k
p
194 20.17 3.86 1087 2.18
Method: sintering again after 860 ℃ of following pre-burnings
Performance: d
33(pC/N) g
33(x10
-3) tg θ (%) ε
T 33/ ε
0k
t/ k
p
146 17.59 4.00 938 1.31
Embodiment four
Prescription: 0.93Bi
0.5Na
0.5TiO
3+ 0.07BaTiO
3+ 0.016wt%In
2O
3
Method: direct sintering
Performance: d
33(pc/N) g
33(x10
-3) tg θ (%) ε
T 33/ ε
0k
t/ k
p
188 22.08 3.55 962 2.08
Method: sintering again after 860 ℃ of following pre-burnings
Performance: d
33(pC/N) g
33(x10
-3) tg θ (%) ε
T 33/ ε
0k
t/ k
p
140 21.01 3.77 753 1.28
Embodiment five
Prescription: 0.93Bi
0.5Na
0.5TiO
3+ 0.07BaTiO
3+ 0.02wt%In
2O
3
Method: direct sintering
Performance: d
33(pC/N) g
33(x10
-3) tg θ (%) ε
T 33/ ε
0k
t/ k
p
172 20.02 3.65 971 0.33
Method: sintering again after 860 ℃ of following pre-burnings
Performance: d
33(pC/N) g
33(x10
-3) tg θ (%) ε
T 33/ ε
0k
t/ k
p
120 15.66 4.06 866 0.31
Claims (2)
1, a kind of no pre-burning bismuth-sodium titanate---barium titanate lead-less piezoelectric ceramic dopant material is characterized in that its composition formula is (1-x) Bi
0.5Na
0.5TiO
3+ xBaTiO
3+ yIn
2O
3, 0.06≤x≤0.08,0≤y≤0.02wt% (wt is weight percentage) wherein.
2, no pre-burning bismuth-sodium titanate according to claim 1---the preparation method of barium titanate lead-less piezoelectric ceramic dopant material direct sintering is as follows:
1) presses general formula (1-x) Bi
0.5Na
0.5TiO
3+ xBaTiO
3+ yIn
2O
3The stoichiometric ratio raw materials weighing,
2) will prepare burden and alcohol by 2g: 1ml puts into nylon ball grinder, dress agate ball in jar, ball milling 4-5 hour, make the batching thorough mixing also levigate,
3) put batching into baking oven, 100 ℃ of oven dry,
4) powder after will drying adds tackiness agent PVA, and thorough mixing is even, and it is 12mm that dry-pressing becomes diameter, and thickness is the disk of 1.3mm,
5) with the disk that presses 550 ℃ of following binder removals 2 hours,
6) treat the disk cool to room temperature after, be warmed up to 800--850 ℃ by 200/ hour again, be incubated 2-3 hour, be warmed up to 1100--1200 ℃ by 150/ hour again, be incubated 1--3 hour, in the temperature-fall period the 900-950 ℃ of insulation of annealing,
7) with silver electrode on the ceramic plate behind the sintering, in 20-100 ℃ silicone oil, with voltage polarizing 5-20 minute of 3-6kV/mm.
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|---|---|---|---|
| CNB2006100182522A CN100357222C (en) | 2006-01-19 | 2006-01-19 | No-prebaking sodium bismuth titanate-barium titanate lead-less piezoelectric ceramic doping material and its prepn |
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|---|---|---|---|
| CNB2006100182522A CN100357222C (en) | 2006-01-19 | 2006-01-19 | No-prebaking sodium bismuth titanate-barium titanate lead-less piezoelectric ceramic doping material and its prepn |
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| Publication Number | Publication Date |
|---|---|
| CN1810714A true CN1810714A (en) | 2006-08-02 |
| CN100357222C CN100357222C (en) | 2007-12-26 |
Family
ID=36843857
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100434394C (en) * | 2007-03-27 | 2008-11-19 | 天津大学 | B-position precursor doped with modified Barium titanate metal composite ceramic and preparation method thereof |
| CN101220511B (en) * | 2007-09-30 | 2011-06-01 | 中国科学院上海硅酸盐研究所 | Method for manufacturing bismuth sodium titanate-barium titanate ferro-electricity single crystal |
| CN108585836A (en) * | 2018-05-22 | 2018-09-28 | 哈尔滨理工大学 | A kind of BNT base piezoelectric ceramics and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4510966B2 (en) * | 1999-11-19 | 2010-07-28 | 日本特殊陶業株式会社 | Piezoelectric ceramics |
| CN1298670C (en) * | 2004-11-02 | 2007-02-07 | 清华大学 | Sodium bismuth phthalate-barium zirconium phthalate leadless piezoelectric ceramic and its preparation method |
-
2006
- 2006-01-19 CN CNB2006100182522A patent/CN100357222C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100434394C (en) * | 2007-03-27 | 2008-11-19 | 天津大学 | B-position precursor doped with modified Barium titanate metal composite ceramic and preparation method thereof |
| CN101220511B (en) * | 2007-09-30 | 2011-06-01 | 中国科学院上海硅酸盐研究所 | Method for manufacturing bismuth sodium titanate-barium titanate ferro-electricity single crystal |
| CN108585836A (en) * | 2018-05-22 | 2018-09-28 | 哈尔滨理工大学 | A kind of BNT base piezoelectric ceramics and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100357222C (en) | 2007-12-26 |
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Granted publication date: 20071226 Termination date: 20100220 |