CN102180670A - Potassium sodium lithium niobate-potassium sodium bismuth titanate lead-free piezoelectric ceramic and preparation method thereof - Google Patents

Potassium sodium lithium niobate-potassium sodium bismuth titanate lead-free piezoelectric ceramic and preparation method thereof Download PDF

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CN102180670A
CN102180670A CN 201110045004 CN201110045004A CN102180670A CN 102180670 A CN102180670 A CN 102180670A CN 201110045004 CN201110045004 CN 201110045004 CN 201110045004 A CN201110045004 A CN 201110045004A CN 102180670 A CN102180670 A CN 102180670A
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piezoelectric ceramic
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potassium sodium
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樊慧庆
陈雷
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Northwestern Polytechnical University
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Abstract

The invention discloses a potassium sodium lithium niobate-potassium sodium bismuth titanate lead-free piezoelectric ceramic and also discloses a preparation method of the potassium sodium lithium niobate-potassium sodium bismuth titanate lead-free piezoelectric ceramic, solving the technical problem that the piezoelectric property of the lead-free piezoelectric ceramic is low. In the technical scheme, the lead-free piezoelectric ceramic with potassium sodium lithium niobate-potassium sodium bismuth titanate is prepared through multi-component doped modification by using a traditional solid phase sintering method, so that the piezoelectric property of the lead-free piezoelectric ceramic is obviously improved, wherein the dielectric constant epsilon33/epsilon 0 of the lead-free piezoelectric ceramic is 425-780, the piezoelectric constant d33 of the lead-free piezoelectric ceramic is 80-235pC/N, the planar electromechanical coupling factor kp of the lead-free piezoelectric ceramic is 24%-40%, the mechanical quality factor Qm of the lead-free piezoelectric ceramic is 20-86, and the Curie temperature Tc of the lead-free piezoelectric ceramic is between 412 DEG C and 482 DEG C; and by using the method, the piezoelectric constant d33 is improved to 162-235 pC/N from 148pC/N in a background art, and the Curie temperature Tc is improved to 412 DEG C-482 DEG C from 395 DEG C in the background art.

Description

Potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics and preparation method thereof
Technical field
The present invention relates to a kind of leadless piezoelectric ceramics, particularly a kind of potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics.The preparation method who also relates to this potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics.
Background technology
Piezoceramic material is widely used in numerous areas such as communication, household electrical appliances, aviation, detection and computer, is a kind of very important function stupalith.But the piezoelectric ceramics that uses on a large scale is lead base piezoelectric ceramics, i.e. two component system PbTiO now 3-PbZrO 3With three component system PbTiO 3-PbZrO 3-ABO 3(ABO 3Be the composite perofskite type ferroelectrics) piezoelectric ceramics.PbO or Pb in the raw material of lead base piezoelectric ceramics 3O 4Account for 70% of total amount, and PbO or Pb 3O 4Volatilization easily in the sintering process of pottery.Contain lead piezoelectric ceramics and producing, brought great harm to physical environment in the discarded and removal process.And the Curie temperature T of this type of piezoelectric ceramics cLower, between 250 ℃～380 ℃.The use temperature of general piezoelectric ceramics is limited in about half of Curie temperature.Therefore they are difficult to satisfied service requirements at high temperature.
Document " Jing-Feng Li and Ke Wang, J.Am.Ceram.Soc.89,706-709 (2006) " has been introduced the K of using plasma electric spark sintering 0.5Na 0.5NbO 3Leadless piezoelectric ceramics.Concrete preparation method is with analytical pure Nb 2O 5, Na 2CO 3, K 2CO 3After the mixing and ball milling 4 hours, calcined 4 hours down at 750 ℃.Then with the incinerating powder as in the graphite box, with plasma agglomeration four minutes.Pottery was 900 ℃ of annealing 1 or 4 hour the most at last.With this kind method agglomerating piezoelectric ceramics performance is d 33=148pC/N, Curie temperature T cIt is 395 ℃.This shows that piezoelectric property is still lower, Curie temperature does not increase substantially than the lead base piezoelectric ceramics, and the using plasma electric spark sintering, so also do not reach the purpose of industrialized production and use.
Summary of the invention
In order to overcome the low deficiency of leadless piezoelectric ceramics piezoelectric property of existing method preparation, the invention provides a kind of potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics.
The present invention also provides the preparation method of this potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics, by the polycomponent doping vario-property, adopt traditional solid-phase sintering method, potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics is provided in preparation, can improve the piezoelectric property of leadless piezoelectric ceramics.
The technical solution adopted for the present invention to solve the technical problems: a kind of potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics, its general formula are (1-x-y-z) K 0.5Na 0.5NbO 3-xLiNbO 3-yBi 0.5Na 0.5TiO 3-zBi 0.5K 0.5TiO 3, in the formula: x is LiNbO 3Molar content, y is Bi 0.5Na 0.5TiO 3Molar content, z is Bi 0.5K 0.5TiO 3Molar content; The range of choice of its numerical value: 0≤x≤0.1,0≤y≤0.05,0≤z≤0.05.
The preparation method of a kind of above-mentioned potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics is characterized in comprising the steps:
(a) with analytical pure Nb 2O 5, Na 2CO 3, K 2CO 3, Li 2CO 3, Bi 2O 3, TiO 2By stoichiometric ratio is (1-x-y-z) K 0.5Na 0.5NbO 3-xLiNbO 3-yBi 0.5Na 0.5TiO 3-z Bi 0.5K 0.5TiO 3Batching, wherein: 0≤x≤0.1,0≤y≤0.05,0≤z≤0.05;
(b) material that will prepare is put into ball grinder in zirconia ball: material: alcohol is 3: 1: 1 ratio batch mixing ball milling, and the ball milling time is 8～12 hours;
The material oven dry back briquetting that (c) will mix, pre-burning is 3～5 hours under 800～900 ℃ of temperature, takes out the incinerating material and smashes, and ball milling is 8～12 hours again, sieves then;
(d) to be pressed into diameter in advance be 12～20mm to the powder after will sieving, and thickness is the disk of 1～1.5mm, at the hydrostatic pressure compacted under of 20～100MPa;
(e) disk after the moulding is incubated 2～4 hours down at 1085～1160 ℃; Sinter into after the porcelain, sanding and polishing, the silver coating slurry under 550～800 ℃, is incubated 20～30 minutes and burns till silver electrode then;
(f) pottery polarized 20～30 minutes in 120 ℃ of silicone oil, and polarized electric field is 3～4kV/mm; Under electric field, be cooled to room temperature, promptly get potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics.
The invention has the beneficial effects as follows: owing to by the polycomponent doping vario-property, adopt traditional solid-phase sintering method, the piezoelectric property that potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics is provided in preparation significantly improves its DIELECTRIC CONSTANT 33/ ε 0Be 425～780, piezoelectric constant d 33Be 80～235pC/N, planar electromechanical coupling factor k pBe 24%～40%, mechanical quality factor Q mBe 20～86, Curie temperature T cBetween 412 ℃～482 ℃.Piezoelectric constant d 33148pC/N by background technology brings up to 162～235pC/N, Curie temperature T cBring up to 412 ℃～482 ℃ by 395 ℃ of background technology.
Below in conjunction with drawings and Examples the present invention is elaborated.
Description of drawings
Fig. 1 is the dielectric thermogram of potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics under different frequency of the embodiment of the invention 1 preparation.
Fig. 2 is the dielectric thermogram of potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics under different frequency of the embodiment of the invention 3 preparations.
Fig. 3 is the potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics surface microstructure photo of the embodiment of the invention 3 preparations.
Fig. 4 is the potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics surface microstructure photo of the embodiment of the invention 5 preparations.
Embodiment
Embodiment 1: with analytical pure Nb 2O 5, Na 2CO 3, K 2CO 3, Li 2CO 3, Bi 2O 3, TiO 2Being base-material, is 0.945K according to stoichiometric ratio 0.5Na 0.5NbO 3-0.05 LiNbO 3-0.004 Bi 0.5Na 0.5TiO 3-0.001Bi 0.5K 0.5TiO 3Proportioning, accurately weighing.Then zirconia ball, material and ethanol were put into the ball grinder ball milling 8 hours according to 3: 1: 1 ratio.With being pressed into sheet after the material oven dry after grinding well, 800 ℃ of following pre-burnings 5 hours.Powder after the calcining is ball milling 8 hours again, sieves then.Powder after sieving, being pressed into diameter in advance is 12mm, thickness is the disk of 1mm, then final molding under the hydrostatic pressure of 20MPa.Disk after the moulding is incubated 2 hours down at 1085 ℃.Sinter into after the porcelain, sanding and polishing, the silver coating slurry under 550 ℃, is incubated 30 minutes and burns till silver electrode then.At last pottery was polarized 20 minutes in 120 ℃ of silicone oil, polarized electric field is 3kV/mm, is cooled to room temperature in silicone oil, takes out ceramic plate then.Piezoelectricity, dielectric properties and Curie temperature see table 1 for details.
As can be seen from Figure 1, the potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics Curie temperature of present embodiment preparation is 482 ℃.
Table 1.
Figure BSA00000436255400031
Embodiment 2: with analytical pure Nb 2O 5, Na 2CO 3, K 2CO 3, Li 2CO 3, Bi 2O 3, TiO 2Being base-material, is 0.94K according to stoichiometric ratio 0.5Na 0.5NbO 3-0.05 LiNbO 3-0.008 Bi 0.5Na 0.5TiO 3-0.002Bi 0.5K 0.5TiO 3Proportioning, accurately weighing.Then zirconia ball, material and ethanol were put into the ball grinder ball milling 9 hours according to 3: 1: 1 ratio.With being pressed into sheet after the material oven dry after grinding well, 820 ℃ of following pre-burnings 5 hours.Powder after the calcining is ball milling 9 hours again, sieves then.Powder after sieving, being pressed into diameter in advance is 20mm, thickness is the disk of 1.4mm, then final molding under the hydrostatic pressure of 40MPa.Disk after the moulding is incubated 2 hours down at 1095 ℃.Sinter into after the porcelain, sanding and polishing, the silver coating slurry under 600 ℃, is incubated 28 minutes and burns till silver electrode then.At last pottery was polarized 22 minutes in 120 ℃ of silicone oil, polarized electric field is 3.2kV/mm, is cooled to room temperature in silicone oil, takes out ceramic plate then.Piezoelectricity, dielectric properties and Curie temperature see table 1 for details.
Embodiment 3: with analytical pure Nb 2O 5, Na 2CO 3, K 2CO 3, Li 2CO 3, Bi 2O 3, TiO 2Being base-material, is 0.935K according to stoichiometric ratio 0.5Na 0.5NbO 3-0.05 LiNbO 3-0.013 Bi 0.5Na 0.5TiO 3-0.002Bi 0.5K 0.5TiO 3Proportioning, accurately weighing.Then zirconia ball, material and ethanol were put into the ball grinder ball milling 10 hours according to 3: 1: 1 ratio.With being pressed into sheet after the material oven dry after grinding well, 840 ℃ of following pre-burnings 4.5 hours.Powder after the calcining is ball milling 10 hours again, sieves then.Powder after sieving, being pressed into diameter in advance is 18mm, thickness is the disk of 1.3mm, then final molding under the hydrostatic pressure of 50MPa.Disk after the moulding is incubated 3 hours down at 1135 ℃.Sinter into after the porcelain, sanding and polishing, the silver coating slurry under 650 ℃, is incubated 26 minutes and burns till silver electrode then.At last pottery was polarized 24 minutes in 120 ℃ of silicone oil, polarized electric field is 3.4kV/mm, is cooled to room temperature in silicone oil, takes out ceramic plate then.Piezoelectricity, dielectric properties and Curie temperature see table 1 for details.
As can be seen from Figure 2, the potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics Curie temperature of present embodiment preparation is 453 ℃.As can be seen from Figure 3, the potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics of present embodiment preparation has tiny cubic type crystal grain, about 1～3 μ m, and the microcosmic pore is less, and the ceramic dense degree has had significant raising.
Embodiment 4: with analytical pure Nb 2O 5, Na 2CO 3, K 2CO 3, Li 2CO 3, Bi 2O 3, TiO 2Being base-material, is 0.93K according to stoichiometric ratio 0.5Na 0.5NbO 3-0.05 LiNbO 3-0.017 Bi 0.5Na 0.5TiO 3-0.003Bi 0.5K 0.5TiO 3Proportioning, accurately weighing.Then zirconia ball, material and ethanol were put into the ball grinder ball milling 11 hours according to 3: 1: 1 ratio.With being pressed into sheet after the material oven dry after grinding well, 860 ℃ of following pre-burnings 4 hours.Powder after the calcining is ball milling 11 hours again, sieves then.Powder after sieving, being pressed into diameter in advance is 14mm, thickness is the disk of 1.1mm, then final molding under the hydrostatic pressure of 60MPa.Disk after the moulding is incubated 3 hours down at 1145 ℃.Sinter into after the porcelain, sanding and polishing, the silver coating slurry under 700 ℃, is incubated 24 minutes and burns till silver electrode then.At last pottery was polarized 26 minutes in 120 ℃ of silicone oil, polarized electric field is 3.6kV/mm, is cooled to room temperature in silicone oil, takes out ceramic plate then.Piezoelectricity, dielectric properties and Curie temperature see table 1 for details.
Embodiment 5: with analytical pure Nb 2O 5, Na 2CO 3, K 2CO 3, Li 2CO 3, Bi 2O 3, TiO 2Being base-material, is 0.93K according to stoichiometric ratio 0.5Na 0.5NbO 3-0.04 LiNbO 3-0.025 Bi 0.5Na 0.5TiO 3-0.005Bi 0.5K 0.5TiO 3Proportioning, accurately weighing.Then zirconia ball, material and ethanol were put into the ball grinder ball milling 12 hours according to 3: 1: 1 ratio.With being pressed into sheet after the material oven dry after grinding well, 880 ℃ of following pre-burnings 3.5 hours.Powder after the calcining is ball milling 12 hours again, sieves then.Powder after sieving, being pressed into diameter in advance is 16mm, thickness is the disk of 1.2mm, then final molding under the hydrostatic pressure of 80MPa.Disk after the moulding is incubated 4 hours down at 1150 ℃.Sinter into after the porcelain, sanding and polishing, the silver coating slurry under 750 ℃, is incubated 22 minutes and burns till silver electrode then.At last pottery was polarized 28 minutes in 120 ℃ of silicone oil, polarized electric field is 3.8kV/mm, is cooled to room temperature in silicone oil, takes out ceramic plate then.Piezoelectricity, dielectric properties and Curie temperature see table 1 for details.
As can be seen from the figure, the potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics of present embodiment preparation has tiny cubic type crystal grain, about 1～2 μ m, and the microcosmic pore is less, and the ceramic dense degree has had significant raising.
Embodiment 6: with analytical pure Nb 2O 5, Na 2CO 3, K 2CO 3, Li 2CO 3, Bi 2O 3, TiO 2Being base-material, is 0.92K according to stoichiometric ratio 0.5Na 0.5NbO 3-0.04 LiNbO 3-0.035 Bi 0.5Na 0.5TiO 3-0.005Bi 0.5K 0.5TiO 3Proportioning, accurately weighing.Then zirconia ball, material and ethanol were put into the ball grinder ball milling 12 hours according to 3: 1: 1 ratio.With being pressed into sheet after the material oven dry after grinding well, 900 ℃ of following pre-burnings 3 hours.Powder after the calcining is ball milling 12 hours again, sieves then.Powder after sieving, being pressed into diameter in advance is 20mm, thickness is the disk of 1.5mm, then final molding under the hydrostatic pressure of 100MPa.Disk after the moulding is incubated 4 hours down at 1160 ℃.Sinter into after the porcelain, sanding and polishing, the silver coating slurry under 800 ℃, is incubated 20 minutes and burns till silver electrode then.At last pottery was polarized 30 minutes in 120 ℃ of silicone oil, polarized electric field is 4kV/mm, is cooled to room temperature in silicone oil, takes out ceramic plate then.Piezoelectricity, dielectric properties and Curie temperature see table 1 for details.
From Fig. 3,4 as can be seen, the potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics of the present invention's preparation has tiny crystal grain and fine and close microtexture.Associative list one is filled a prescription as can be seen and is 0.94K 0.5Na 0.5NbO 3-0.05LiNbO 3-0.008 Bi 0.5Na 0.5TiO 3-0.002Bi 0.5K 0.5TiO 3Piezoelectric ceramics have optimum properties, not only have high Curie temperature, also have excellent piezoelectric property simultaneously, improved the working temperature of piezoelectric ceramics.
In a word, the present invention is by the polycomponent doping vario-property, with traditional solid-phase sintering method, cheap Costco Wholesale is successfully prepared the multi constituent niobate high-temp leadless piezoelectric ceramics with excellent piezoelectric property, and therefore leadless piezoelectric ceramics of the present invention is fit to industrialization promotion and scale operation.

Claims (2)

1. potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics, its general formula is (1-x-y-z) K 0.5Na 0.5NbO 3-xLiNbO 3-yBi 0.5Na 0.5TiO 3-zBi 0.5K 0.5TiO 3, in the formula: x is LiNbO 3Molar content, y is Bi 0.5Na 0.5TiO 3Molar content, z is Bi 0.5K 0.5TiO 3Molar content; The range of choice of its numerical value: 0≤x≤0.1,0≤y≤0.05,0≤z≤0.05.
2. the preparation method of the described potassium-sodium niobate lithium of claim 1-bismuth sodium potassium titanate leadless piezoelectric ceramics is characterized in that comprising the steps:
(a) with analytical pure Nb 2O 5, Na 2CO 3, K 2CO 3, Li 2CO 3, Bi 2O 3, TiO 2By stoichiometric ratio is (1-x-y-z) K 0.5Na 0.5NbO 3-xLiNbO 3-yBi 0.5Na 0.5TiO 3-z Bi 0.5K 0.5TiO 3Batching, wherein: 0≤x≤0.1,0≤y≤0.05,0≤z≤0.05;
(b) material that will prepare is put into ball grinder in zirconia ball: material: alcohol is 3: 1: 1 ratio batch mixing ball milling, and the ball milling time is 8～12 hours;
The material oven dry back briquetting that (c) will mix, pre-burning is 3～5 hours under 800～900 ℃ of temperature, takes out the incinerating material and smashes, and ball milling is 8～12 hours again, sieves then;
(d) to be pressed into diameter in advance be 12～20mm to the powder after will sieving, and thickness is the disk of 1～1.5mm, at the hydrostatic pressure compacted under of 20～100MPa;
(e) disk after the moulding is incubated 2～4 hours down at 1085～1160 ℃; Sinter into after the porcelain, sanding and polishing, the silver coating slurry under 550～800 ℃, is incubated 20～30 minutes and burns till silver electrode then;
(f) pottery polarized 20～30 minutes in 120 ℃ of silicone oil, and polarized electric field is 3～4kV/mm; Under electric field, be cooled to room temperature, promptly get potassium-sodium niobate lithium-bismuth sodium potassium titanate leadless piezoelectric ceramics.
CN 201110045004 2011-02-24 2011-02-24 Potassium sodium lithium niobate-potassium sodium bismuth titanate lead-free piezoelectric ceramic and preparation method thereof Pending CN102180670A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503413A (en) * 2011-10-18 2012-06-20 同济大学 Textured (1-x-y) BNT-xBKT-yKNN ceramic material and preparation method thereof
CN108467263A (en) * 2018-03-19 2018-08-31 聊城大学 A kind of rear-earth-doped bismuth-sodium titanate base ceramics and preparation method and the electric field adjusting method for adjusting piezoelectric property and luminescent properties simultaneously
CN111151434A (en) * 2020-02-29 2020-05-15 桐乡清锋科技有限公司 Low-frequency leadless piezoelectric atomization element
CN113582685A (en) * 2021-08-05 2021-11-02 湖南省美程陶瓷科技有限公司 Lead-free piezoelectric ceramic material for breathing machine and preparation method thereof
CN114907122A (en) * 2022-04-01 2022-08-16 贵州理工学院 Calcium zirconate-sodium bismuth titanate-sodium lithium sodium potassium antimonate lead-free piezoelectric ceramic and preparation method thereof
CN116477944A (en) * 2022-12-02 2023-07-25 湖南大学 Potassium sodium niobate-based leadless piezoelectric ceramic and preparation method and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101337815A (en) * 2008-08-13 2009-01-07 西北工业大学 Leadless piezoelectric ceramics and method for preparing the same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101337815A (en) * 2008-08-13 2009-01-07 西北工业大学 Leadless piezoelectric ceramics and method for preparing the same

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102503413A (en) * 2011-10-18 2012-06-20 同济大学 Textured (1-x-y) BNT-xBKT-yKNN ceramic material and preparation method thereof
CN102503413B (en) * 2011-10-18 2013-05-01 同济大学 Textured (1-x-y) BNT-xBKT-yKNN ceramic material and preparation method thereof
CN108467263A (en) * 2018-03-19 2018-08-31 聊城大学 A kind of rear-earth-doped bismuth-sodium titanate base ceramics and preparation method and the electric field adjusting method for adjusting piezoelectric property and luminescent properties simultaneously
CN108467263B (en) * 2018-03-19 2021-07-13 聊城大学 Rare earth doped sodium bismuth titanate-based ceramic, preparation method thereof and electric field adjusting method for simultaneously adjusting piezoelectric property and luminescence property
CN111151434A (en) * 2020-02-29 2020-05-15 桐乡清锋科技有限公司 Low-frequency leadless piezoelectric atomization element
CN113582685A (en) * 2021-08-05 2021-11-02 湖南省美程陶瓷科技有限公司 Lead-free piezoelectric ceramic material for breathing machine and preparation method thereof
CN113582685B (en) * 2021-08-05 2022-07-15 湖南省美程陶瓷科技有限公司 Lead-free piezoelectric ceramic material for breathing machine and preparation method thereof
CN114907122A (en) * 2022-04-01 2022-08-16 贵州理工学院 Calcium zirconate-sodium bismuth titanate-sodium lithium sodium potassium antimonate lead-free piezoelectric ceramic and preparation method thereof
CN116477944A (en) * 2022-12-02 2023-07-25 湖南大学 Potassium sodium niobate-based leadless piezoelectric ceramic and preparation method and application thereof

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