CN1285539C - Bismuth sodium titanate-barium titanate base piezoelectric ceramic and its prepn process - Google Patents
Bismuth sodium titanate-barium titanate base piezoelectric ceramic and its prepn process Download PDFInfo
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- CN1285539C CN1285539C CN200510041601.8A CN200510041601A CN1285539C CN 1285539 C CN1285539 C CN 1285539C CN 200510041601 A CN200510041601 A CN 200510041601A CN 1285539 C CN1285539 C CN 1285539C
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- titanate
- barium
- piezoelectric ceramics
- barium titanate
- bismuth
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- 239000000919 ceramic Substances 0.000 title claims abstract description 31
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910002113 barium titanate Inorganic materials 0.000 title claims description 17
- 238000000034 method Methods 0.000 title abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 25
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 22
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011734 sodium Substances 0.000 claims abstract description 17
- 229910052709 silver Inorganic materials 0.000 claims abstract description 15
- 239000004332 silver Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 13
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims abstract description 11
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 11
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 11
- 238000005096 rolling process Methods 0.000 claims abstract description 8
- 239000003292 glue Substances 0.000 claims abstract description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 16
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 14
- 239000011230 binding agent Substances 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 11
- 235000017550 sodium carbonate Nutrition 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000007858 starting material Substances 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 230000005684 electric field Effects 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 229920002545 silicone oil Polymers 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 229910010252 TiO3 Inorganic materials 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 238000012769 bulk production Methods 0.000 abstract 1
- 238000013329 compounding Methods 0.000 abstract 1
- 238000003801 milling Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 abstract 1
- 238000003825 pressing Methods 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 229910001887 tin oxide Inorganic materials 0.000 abstract 1
- 230000010287 polarization Effects 0.000 description 9
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 5
- 230000008878 coupling Effects 0.000 description 5
- 238000010168 coupling process Methods 0.000 description 5
- 238000005859 coupling reaction Methods 0.000 description 5
- 235000015895 biscuits Nutrition 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
The present invention discloses sodium bismuth titanate-barium titanate group piezoelectric ceramics which comprise bismuth trioxide, sodium carbonate, barium carbonate, titanium dioxide and tin oxide, and have the chemical composition of (1-x)((Na<0.5>Bi<0.5>)TiO3)-xBaTiO3-ySnO2, wherein x is more than 0 and less than 0.1, and y is more than 0 and less than 10. The present invention also discloses a method for preparing the sodium bismuth titanate-barium titanate group piezoelectric ceramics, which comprises the steps: square tablets are finally formed by compounding materials, vibration milling, mixing, pressing blocks, presintering, adding adhesive, and rolling on a roller mill again and again, the square tablets are put in a baking oven to be dried into plain tablets, and the sodium bismuth titanate-barium titanate group piezoelectric ceramics are finally formed by eliminating glue, sintering, burning silver, and polarizing in silicon oil. Because different doped elements and different element proportions are adopted, the coercive field and the resistivity of the piezoelectric ceramics are effectively reduced, and a polarizing technology is simple and easy. The method of the present invention can prepare leadless piezoelectric ceramics with different piezoelectric property and dielectric property which can satisfy the requirements of different fields. The piezoelectric ceramics of the present invention adopt industrial roll forming, have simple method and low cost, and are suitable for bulk production.
Description
Technical field
The present invention relates to a kind of bismuth sodium titanate-barium titanate base piezoelectric ceramic, also relate to the preparation method of bismuth sodium titanate-barium titanate base piezoelectric ceramic.
Background technology
Piezoelectric ceramics can produce strain under the extra electric field effect, simultaneously, under external force, piezoelectric ceramics can produce electric charge at the two poles of the earth, therefore is widely used in fields such as micro positioner, transmitter, resonator, transverter and wave filter.
Document " G.A.Smolensky; V.A.Isupov; A.I.agranovskaya; N.N.Krainik; Sov.Phys.-SolidState (Engl.Transl.) 2 (11) (1961) 2651-2654 " has been introduced the bismuth-sodium titanate of inventions such as G.A.Smolensky, it is a kind of composite perofskite ferroelectrics, is trigonal system during room temperature, and Curie temperature is 320 ℃.It is strong that bismuth-sodium titanate has ferroelectricity, remnant polarization P
r=38 μ C/cm
2, piezo-electric modulus is big, thickness electromechanical coupling coefficient k
tGood characteristic such as be about 0.40~0.50, specific inductivity is little, acoustical behavior is good, and sintering temperature is low, but bismuth-sodium titanate pottery coercive field is very high, is about 73kV/cm, and very high in the ferroelectric phase region specific conductivity, thereby be difficult to polarization, performance also is difficult to be improved.
Barium titanate is the leadless piezoelectric ceramics of large-scale production, but the piezoelectric constant d of barium titanate
33About 100pC/N, be difficult to improve its performance significantly, to satisfy different needs by mixing; The working temperature district is narrower, is about 10~70 ℃, and Curie temperature is 120 ℃, has phase transformation near 0 ℃, causes the temperature stability of performance perameter not good enough.
For the bismuth-sodium titanate pottery of mixing barium titanate, in the electric property of having reported, piezoelectric constant d
33Be about 100pC/N, planar electromechanical coupling factor kp is about 0.18, and quality factor q m is about 122, can not satisfy the demand of actual use.
Summary of the invention
For overcome in the prior art bismuth-sodium titanate pottery coercive field height, specific conductivity is high and be difficult to polarization, barium titanate ceramics working temperature district is narrow to be waited not enoughly, the invention provides a kind of bismuth sodium titanate-barium titanate base piezoelectric ceramic, adopts tin, mn ion to Bi
1/2Na
1/2TiO
3-BaTiO
3Carry out separately with composite mixed, to reduce its coercive field and specific conductivity.
The present invention also provides the preparation method of this bismuth sodium titanate-barium titanate base piezoelectric ceramic.
Technical scheme of the present invention is:
A kind of bismuth sodium titanate-barium titanate base piezoelectric ceramic, its starting material are bismuthous oxide bismuth trioxide, yellow soda ash, barium carbonate, titanium dioxide, stannic oxide, and stoichiometric ratio is (1-x) [(Na
0.5Bi
0.5) TiO
3]-xBaTiO
3-ywt%SnO
2
Wherein: 0<x<0.1,0<y<10.
Described starting material are bismuthous oxide bismuth trioxide, yellow soda ash, barium carbonate, titanium dioxide, stannic oxide, Manganse Dioxide, and stoichiometric ratio is (1-x) [(Na
0.5Bi
0.5) TiO
3]-xBaTiO
3-ywt%SnO
2-zwt%MnO
2
Wherein: 0<x<0.1,0<y<10,0≤z<10.
A kind of above-mentioned bismuth sodium titanate-barium titanate base piezoelectric ceramic preparation method,
(1) be (1-x) [(Na with starting material bismuthous oxide bismuth trioxide, yellow soda ash, barium carbonate, titanium dioxide, stannic oxide by stoichiometric ratio
0.5Bi
0.5) TiO
3]-xBaTiO
3-ywt%SnO
2Batching, wherein: 0<x<0.1,0<y<10;
(2) material that will prepare is put into the vibration hopper in iron ball: material is 3: 1 a ratio batch mixing, and the time of vibration is 6~12 hours;
The material briquetting that (3) will mix, pre-burning is 1~2 hour under 800~900 ℃ of temperature, takes out the incinerating material and smashes, and vibration was sieved after 6~12 hours again;
(4) binding agent of adding 20~28wt%, repeat-rolling is 1~2 hour on roll forming machine, and final molding is 12 * 12 * 0.5mm
3Square sheet;
(5) the square sheet of moulding is put into 120 ℃ in baking oven and be dried into plain sheet in 10~13 hours, the plain sheet that to dry is then put into the stove binder removal, temperature rise rate is 30 ℃/h in the time of 25~500 ℃, in the time of 500~800 ℃ 100 ℃/h, and be incubated 2~4 hours, furnace cooling at 270 ℃, 360 ℃, 500 ℃ and 800 ℃ respectively;
(6) the plain sheet of having arranged glue is put into sintering oven, and sintering in 1100~1200 ℃ of temperature ranges takes out after sintering is finished, coating low-temperature silver slurry, and 800 ℃ of silver ink firings become electrode;
(7) ceramics that will apply silver electrode immerses in 25 ℃ of silicone oil and polarized 10~30 minutes, and polarized electric field is 3~5kV/mm.
Comprise Manganse Dioxide in the described starting material, its stoichiometric ratio is (1-x) [(Na
0.5Bi
0.5) TiO
3]-xBaTiO
3-ywt%SnO
2-zwt%MnO
2, wherein: 0<x<0.1,0<y<10,0≤z<10.
The invention has the beneficial effects as follows: owing to adopted different doped elements and different element proportionings, effectively reduced the coercive field and the resistivity of piezoelectric ceramics, made polarization process simple.The inventive method can prepare the leadless piezoelectric ceramics of different piezoelectricity, dielectric properties, thereby satisfies the user demand of different field; In the process of ceramic plate moulding, adopted industrialized rolling formation, technical process is simple, good reproducibility, equipment requirements is low, makes to be fit to extensive, mass production by low production cost.The resulting electrical parameter of the present invention is piezoelectric constant d
33Be 80~125pC/N, plane coupling electromechanical coefficient kp is 0.17~0.25, and quality factor q m is 40~163, and thickness electromechanical coupling coefficient kt is 0.39~0.51, than the bismuth-sodium titanate piezoelectric ceramics constant d that mixes barium titanate of prior art for preparing
33=100pC/N, planar electromechanical coupling factor kp=0.18, big many of quality factor q m=122.
The present invention is further described below in conjunction with drawings and Examples.
Description of drawings
Fig. 1 is a plain sheet binder removal artwork of the present invention
Fig. 2 is ceramic sintering process figure of the present invention
Fig. 3 is 0.96[(Na
0.5Bi
0.5) TiO
3]-0.04BaTiO
3-0.2wt%SnO
2At 1110 ℃ of sintered surface microstructure photos
Fig. 4 is 0.94[(Na
0.5Bi
0.5) TiO
3]-0.06BaTiO
3-0.4wt%MnO
2-0.2wt%SnO
2At 1110 ℃ of sintered surface microstructure photos
Embodiment
Embodiment 1, is that 99.0% bismuthous oxide bismuth trioxide, content are that 99.8% yellow soda ash, content are that 99.0% barium carbonate, content are that 98% titanium dioxide, content are 99.5% stannic oxide with analytical pure level content, is 0.96[(Na by stoichiometric ratio
0.5Bi
0.5) TiO
3]-0.04BaTiO
3-0.2wt%SnO
2Carry out weigh batching.The material for preparing is put into the vibration hopper in iron ball: material is 3: 1 a ratio batch mixing, does not add other media in the batch mixing process.The time of vibration is 6 hours, and the material briquetting that mixes pre-burning 1 hour under 800 ℃ of temperature is taken out the incinerating material and smashed, and vibration was sieved after 6 hours again; Add the binding agent of 20wt%, repeat-rolling is 1 hour on roll forming machine, and final molding is 12 * 12 * 0.5mm
3Square sheet, put into 120 ℃ in baking oven and be dried into plain sheet in 10 hours, the plain sheet that will dry is then put into the stove binder removal, temperature rise rate is 30 ℃/h in the time of 25~500 ℃, be 100 ℃/h in the time of 500~800 ℃, and be incubated 2 hours, furnace cooling at 270 ℃, 360 ℃, 500 ℃ and 800 ℃ respectively; Arranged the plain sheet of glue and put into sintering oven,, taken out after sintering is finished at 1100 ℃ of sintering, temperature silver slurry in the coating, 800 ℃ of silver ink firings become electrode, and polarization is 10 minutes in 25 ℃ silicone oil, and polarized electric field is 3kV/mm.First row during its electric property is seen attached list.
Subordinate list
Group | Density | kp | Qm | εr | kt | Nd | tanδ |
Embodiment 1 | 5.77 5.45 5.41 5.77 | 0.22 0.17 0.19 0.25 | 40 51 154 163 | 804 1237 567 627 | 0.39 0.45 0.46 0.51 | 2306 2390 2558 2453 | 0.025 0.019 0.0065 0.0061 |
Embodiment 3, are that 99.0% bismuthous oxide bismuth trioxide, content are that 99.8% yellow soda ash, content are that 99.0% barium carbonate, content are that 98% titanium dioxide, content are 99.5% stannic oxide with analytical pure level content, are 0.92[(Na by stoichiometric ratio
0.5Bi
0.5) TiO
3]-0.08BaTiO
3-0.2wt%SnO
2Carry out weigh batching.The material for preparing is put into the vibration hopper in iron ball: material is 3: 1 a ratio batch mixing, does not add other media in the batch mixing process.The time of vibration is 10 hours, and the material briquetting that mixes pre-burning 2 hours under 850 ℃ of temperature is taken out the incinerating material and smashed, and vibration was sieved after 10 hours again; Add the binding agent of 25wt%, repeat-rolling is 2 hours on roll forming machine, and final molding is 12 * 12 * 0.5mm
3Square sheet, put into 120 ℃ in baking oven and be dried into plain sheet in 12 hours, the plain sheet that will dry is then put into the stove binder removal, temperature rise rate is 30 ℃/h in the time of 25~500 ℃, be 100 ℃/h in the time of 500~800 ℃, and be incubated 2 hours, furnace cooling at 270 ℃, 360 ℃, 500 ℃ and 800 ℃ respectively; Arranged the biscuit of glue and put into sintering oven,, taken out after sintering is finished at 1150 ℃ of sintering, temperature silver slurry in the coating, 800 ℃ of silver ink firings become electrode, and polarization is 20 minutes in 25 ℃ silicone oil, and polarized electric field is 4kV/mm.Its electric property middle the third line of seeing attached list.
From Fig. 3, Fig. 4 as can be seen, along with the variation of proportioning, the microstructure of piezoelectric ceramics, the quantity of pore and size, small variation takes place in the size of crystal grain and shape, in conjunction with subordinate list as can be seen, prescription 0.94[(Na
0.5Bi
0.5) TiO
3]-0.06BaTiO
3-0.4wt%MnO
2-0.2wt%SnO
2Can obtain the good comprehensive piezoelectric property at 1110 ℃.
In a word, the present invention is by reasonable raw material proportioning, doping vario-property, optimization preparation, sintering and polarization process, realized the preparation of industrialization of the bismuth-sodium titanate base lead-free piezoelectric ceramic of, excellent property good with environment compatibility.
Claims (4)
1, a kind of bismuth sodium titanate-barium titanate base piezoelectric ceramic, its starting material are bismuthous oxide bismuth trioxide, yellow soda ash, barium carbonate, titanium dioxide, stannic oxide, stoichiometric ratio is (1-x) [(Na
0.5Bi
0.5) TiO
3]-xBaTiO
3-ywt%SnO
2
Wherein: 0<x<0.1,0<y<10.
2, bismuth sodium titanate-barium titanate base piezoelectric ceramic according to claim 1 is characterized in that: described starting material are bismuthous oxide bismuth trioxide, yellow soda ash, barium carbonate, titanium dioxide, stannic oxide, Manganse Dioxide, and stoichiometric ratio is (1-x) [(Na
0.5Bi
0.5) TiO
3]-xBaTiO
3-ywt%SnO
2-zwt%MnO
2
Wherein: 0<x<0.1,0<y<10,0≤z<10.
3, a kind of bismuth sodium titanate-barium titanate base piezoelectric ceramic preparation method according to claim 1,
(1) be (1-x) [(Na with starting material bismuthous oxide bismuth trioxide, yellow soda ash, barium carbonate, titanium dioxide, stannic oxide by stoichiometric ratio
0.5Bi
0.5) TiO
3]-xBaTiO
3-ywt%SnO
2Batching, wherein: 0<x<0.1,0<y<10;
(2) material that will prepare is put into the vibration hopper in iron ball: material is 3: 1 a ratio batch mixing, and the time of vibration is 6~12 hours;
The material briquetting that (3) will mix, pre-burning is 1~2 hour under 800~900 ℃ of temperature, takes out the incinerating material and smashes, and vibration was sieved after 6~12 hours again;
(4) binding agent of adding 20~28wt%, repeat-rolling is 1~2 hour on roll forming machine, and final molding is 12 * 12 * 0.5mm
3Square sheet;
(5) the square sheet of moulding is put into 120 ℃ in baking oven and be dried into plain sheet in 10~13 hours, the plain sheet that to dry is then put into the stove binder removal, temperature rise rate is 30 ℃/h in the time of 25~500 ℃, in the time of 500~800 ℃ 100 ℃/h, and be incubated 2~4 hours, furnace cooling at 270 ℃, 360 ℃, 500 ℃ and 800 ℃ respectively;
(6) the plain sheet of having arranged glue is put into sintering oven, and sintering in 1100~1200 ℃ of temperature ranges takes out after sintering is finished, coating low-temperature silver slurry, and 800 ℃ of silver ink firings become electrode;
(7) ceramics that will apply silver electrode immerses in 25 ℃ of silicone oil and polarized 10~30 minutes, and polarized electric field is 3~5kV/mm.
4, bismuth sodium titanate-barium titanate base piezoelectric ceramic preparation method according to claim 3, it is characterized in that: comprise Manganse Dioxide in the described starting material, its stoichiometric ratio is: (1-x) [(Na
0.5Bi
0.5) TiO
3]-xBaTiO
3-ywt%SnO
2-zwt%MnO
2, wherein: 0<x<0.1,0<y<10,0≤z<10.
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US11538632B2 (en) | 2021-01-29 | 2022-12-27 | Samsung Electronics Co., Ltd. | Dielectric material, method of preparing the same, and device comprising the dielectric material |
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DE102009035425A1 (en) * | 2009-07-31 | 2011-02-17 | Epcos Ag | Piezoelectric ceramic composition, process for the preparation of the composition and electrical component, comprising the composition |
CN102173784B (en) * | 2011-01-21 | 2012-12-19 | 天津大学 | Method for preparing sodium bismuth titanate-barium titanate composite dielectric ceramic through sol cladding method |
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