CN101891474A - Potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics and preparation method thereof - Google Patents
Potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics and preparation method thereof Download PDFInfo
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Abstract
The invention discloses potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics and a preparation method thereof. The chemical composition general formula of the potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics is (1-x)K0.5Na0.5NbO3-xBi0.5(K0.82Na0.18)TiO3, wherein x is more than 0 and less than 0.2 and the x is molar fraction. The method comprises the following steps of: proportioning potassium carbonate, sodium carbonate, titanium dioxide, niobium pentaoxide and bismuth trioxide according to a stoichiometric ratio (1-x)K0.5Na0.5NbO3-xBi0.5(K0.82Na0.18)TiO3 (x is more than 0 and less than 0.2 and the x is molar fraction), then performing processes of ball milling, calcining, secondary ball milling, granulation, shaping, gel removal, high temperature sintering and the like, and finally preparing the potassium-sodium niobate-sodium potassium bismuth titanate-based lead-free piezoelectric ceramics with high piezoelectric performance. The method greatly improves the piezoelectric performance of the lead-free piezoelectric ceramics system, improves the process stability of the materials, and ensures that the lead-free piezoelectric ceramics of the potassium-sodium niobate system achieves a practical level on two aspects of components and processes.
Description
Technical field
The present invention relates to a kind of potassium-sodium niobate-sodium potassium bismuth titanate leadless piezoelectric ceramics and preparation method thereof, belong to electronic ceramic fields.
Background technology
Potassium niobate sodium-based leadless piezoelectric ceramic has low density, high acoustic velocity, and characteristics such as mechanical quality factor and piezoelectric constant span broad are considered to be expected to most replace the material of lead base piezoelectric ceramics.How accurate homotype phase boundary compounding technology is the effective ways that improve the material piezoelectric property at present.Document " Atsushi Sasaki, Tatsuya Chiba, Youichi Mamiya and Etsuo Otsuki, Dielectric and Piezoelectric Properties of (Bi
0.5Na
0.5) TiO
3-(Bi
0.5K
0.5) TiO
3Systems, Jpn.J.Appl.Phys.38 (1999) pp.5564-5567 " provided Bi
0.5Na
0.5) TiO
3-(Bi
0.5K
0.5) TiO
3Accurate homotype phase boundary.The present invention adopts K
0.5Na
0.5NbO
3With Bi
0.5Na
0.5) TiO
3-(Bi
0.5K
0.5) TiO
3Accurate homotype phase boundary compounding technology, with salt of wormwood, yellow soda ash, Niobium Pentxoxide, titanium dioxide, bismuthous oxide bismuth trioxide is raw material, prepare the potassium-sodium niobate-sodium potassium bismuth titanate leadless piezoelectric ceramics with traditional solid phase reaction method, method is simple, cost is low, is suitable for the application of large-scale industrialization production and piezo component.
Summary of the invention
The object of the invention is to provide a kind of potassium-sodium niobate-sodium potassium bismuth titanate leadless piezoelectric ceramics and preparation method thereof.Particularly in the potassium-sodium niobate-sodium potassium bismuth titanate binary system, determine accurate homotype phase boundary, the different piezoelectricity of acquisition, dielectric, electromechanical coupling characteristics.Make the piezoelectric constant of the system solid solution of potassium-sodium niobate-sodium potassium bismuth titanate improve 1 to 2 times than pure potassium-sodium niobate.
Potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics chemical constitution general formula of the present invention is: (1-x) K
0.5Na
0.5NbO
3-xBi
0.5(K
0.82Na
0.18) TiO
3, wherein: 0＜x＜0.20.With the synthetic piezoelectric ceramics of solid reaction process preparation.
Concrete steps are as follows:
(1), be (1-x) K by stoichiometric ratio with salt of wormwood, yellow soda ash, titanium dioxide, bismuthous oxide bismuth trioxide, Niobium Pentxoxide
0.5Na
0.5NbO
3-xBi
0.5(K
0.82Na
0.18) TiO
3Batching, wherein: 0＜x＜0.2;
(2) material that step (1) is prepared is put into the ball mill batch mixing, and ball/material mass ratio is 2～20, and the material of ball is a kind of in iron ball, agate ball, zirconia ball and the alumina balls, and the time of ball milling is 6～14 hours, and rotating speed is 200～450 rev/mins;
(3) the material briquetting that step (2) is mixed, pre-burning is 1～3 hour under 900～1300 ℃ of temperature, and take out the incinerating material and grind, ball milling once more, ball milling time and synchronization rapid (2), powder is crossed 40 mesh sieves then, and the material of ball and ball/material are than same step (2);
(4) powder that step (3) is obtained adds the pure water of its mass ratio 10-45%, the polyacrylic acid ammonia dispersion agent of mass ratio 0.2～2% and the poly (vinyl alcohol) binder of mass ratio 0.2～2%, mixed in 1～3 hour through ball milling and to form slip, ball milling speed is 50～300 rev/mins, adopt the air-stream spraying granulation, obtain particle diameter and be 0.01～1 millimeter potassium-sodium niobate-sodium potassium bismuth titanate powder granule;
(5) powder granule that step (4) is made is put into press, suppresses disk or square sheet under the pressure of 200～900MPa;
(6) disk of step (5) moulding or square sheet are put into 120 ℃ of bakings of baking oven and became plain sheet in 1～6 hour, the plain sheet that to dry is then put into the stove binder removal, temperature rise rate is 30～90 ℃/h at 25～500 ℃ of temperature sections, 500～800 ℃ of temperature sections are 90～120 ℃/h, and be incubated 1～4 hour, furnace cooling at 270 ℃, 360 ℃, 500 ℃ and 800 ℃ respectively;
(7) the plain sheet that step (6) is obtained is put into sintering oven, rises to 1100～1500 ℃ with 2～12 ℃/minute temperature rise rates, is incubated 1～8 hour, and furnace cooling makes potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics then.
The inventive method improved greatly the leadless piezoelectric ceramics system piezoelectric property, improved the technology stability of material, make the leadless piezoelectric ceramics of potassium-sodium niobate system reach the practicability level from composition and technology two aspects.
Description of drawings
Fig. 1 is 0.97K for component of the present invention
0.5Na
0.5NbO
3-0.03Bi
0.5(K
0.82Na
0.18) TiO
3The XRD spectrum of pottery.
Fig. 2 is 0.91K for component of the present invention
0.5Na
0.5NbO
3-0.09Bi
0.5(K
0.82Na
0.18) TiO
3The SEM figure of pottery.
Embodiment
Further illustrate substantive distinguishing features of the present invention and significant advantage below by embodiment, the present invention only is confined to described embodiment by no means.
Embodiment 1:
Is 0.95K with yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide, Niobium Pentxoxide by stoichiometric ratio with conventional solid-state method
0.5Na
0.5NbO
3-0.05Bi
0.5(K
0.82Na
0.18) TiO
3Batching.Raw material is put into ball grinder in zirconia ball: the material mass ratio is 5: 1 a ratio batch mixing.The time of ball milling is 12 hours, and rotating speed is 400 rev/mins, and the material briquetting that mixes pre-burning 2 hours under 950 ℃ of temperature is taken out the incinerating material and ground, and ball milling is crossed 40 mesh sieves after 12 hours again, and rotational speed of ball-mill is 400 rev/mins; Powder is added the pure water of its mass ratio 32%, the polyacrylic acid ammonia dispersion agent of mass ratio 1.2% and the poly (vinyl alcohol) binder of mass ratio 0.8%, mixed in 2 hours through ball milling and form slip, ball milling speed is 100 rev/mins, adopts the air-stream spraying granulation; Powder granule is put into press, obtains the disk of 1.2 millimeters of 15 millimeters thickness of diameter under 450MPa pressure; Put into 120 ℃ of bakings of baking oven and became plain sheet in 10 hours, the plain sheet that to dry is then put into the stove binder removal, and temperature rise rate is 30 ℃/h at 25～500 ℃ of temperature sections, and 500～800 ℃ of temperature sections are 100 ℃/h, 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, temperature rise rate is 5 ℃/minute, at 1150 ℃ of sintering, then furnace cooling.Sintering takes out after finishing, and temperature silver slurry became electrode in 0.5 hour 800 ℃ of insulations in the coating, and polarization is 10 minutes in 25 ℃ silicone oil, and polarized electric field is 1kV/mm.The potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics constant d that adopts this method to obtain
33Be 280pC/N, plane coupling electromechanical coefficient k
pBe 0.54, quality factor q
mBe 721, thickness electromechanical coupling coefficient k
tBe 0.67.
Embodiment 2:
Is 0.97K with yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide, Niobium Pentxoxide by stoichiometric ratio with conventional solid-state method
0.5Na
0.5NbO
3-0.03Bi
0.5(K
0.82Na
0.18) TiO
3Batching.Raw material is put into ball grinder in zirconia ball: material is 10: 1 a ratio batch mixing, does not add other media in the batch mixing process.The time of ball milling is 8 hours, and rotating speed is 350 rev/mins, and the material briquetting that mixes pre-burning 2 hours under 1000 ℃ of temperature is taken out the incinerating material and ground, and ball milling is crossed 40 mesh sieves after 8 hours again, and rotational speed of ball-mill is 350 rev/mins; Powder is added the pure water of its mass ratio 20%, the polyacrylic acid ammonia dispersion agent of mass ratio 1.6% and the poly (vinyl alcohol) binder of mass ratio 0.5%, mixed in 2 hours through ball milling and form slip, ball milling speed is 150 rev/mins, adopts the air-stream spraying granulation; Powder granule is put into press, obtains the disk of 1.2 millimeters of 15 millimeters thickness of diameter under 500MPa pressure; Put into 120 ℃ of bakings of baking oven and became plain sheet in 8 hours, the plain sheet that to dry is then put into the stove binder removal, and temperature rise rate is 30 ℃/h at 25～500 ℃ of temperature sections, and 500～800 ℃ of temperature sections are 100 ℃/h, and be incubated 1 hour, furnace cooling at 270 ℃, 360 ℃, 500 ℃ and 800 ℃ respectively; Arranged the plain sheet of glue and put into sintering oven, temperature rise rate is 10 ℃/minute, at 1250 ℃ of sintering, then furnace cooling.Temperature silver slurry became electrode in 0.5 hour 800 ℃ of insulations in the coating, and polarization is 30 minutes in 25 ℃ silicone oil, and polarized electric field is 1.5kV/mm.The potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics constant d that adopts this method to obtain
33Be 373pC/N, plane coupling electromechanical coefficient k
pBe 0.64, quality factor q
mBe 558, thickness electromechanical coupling coefficient k
tBe 0.77.Fig. 1 has provided the XRD figure spectrum of bismuth potassium titanate sodium potassium-sodium niobate pottery.
Embodiment 3:
Is 0.85K with yellow soda ash, salt of wormwood, titanium dioxide, bismuthous oxide bismuth trioxide, Niobium Pentxoxide by stoichiometric ratio with conventional solid-state method
0.5Na
0.5NbO
3-0.15Bi
0.5(K
0.82Na
0.18) TiO
3Batching.Raw material is put into ball grinder in zirconia ball: material is 15: 1 a ratio batch mixing, does not add other media in the batch mixing process.The time of ball milling is 10 hours, and rotating speed is 450 rev/mins, and the material briquetting that mixes pre-burning 2 hours under 1200 ℃ of temperature is taken out the incinerating material and ground, and ball milling is crossed 40 mesh sieves after 10 hours again, and rotational speed of ball-mill is 450 rev/mins; Powder is added the pure water of its mass ratio 40%, the polyacrylic acid ammonia dispersion agent of mass ratio 1% and the poly (vinyl alcohol) binder of mass ratio 1.5%, mixed in 2 hours through ball milling and form slip, ball milling speed is 80 rev/mins, adopts the air-stream spraying granulation; Powder granule is put into press, obtains the disk of 1.2 millimeters of 15 millimeters thickness of diameter under 350MPa pressure; Put into 120 ℃ of bakings of baking oven and became plain sheet in 10 hours, the plain sheet that to dry is then put into the stove binder removal, and temperature rise rate is 30 ℃/h in the time of 25～500 ℃, is 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, temperature rise rate is 7 ℃/minute, at 1320 ℃ of sintering, then furnace cooling.Sintering takes out after finishing, and temperature silver slurry became electrode in 0.5 hour 800 ℃ of insulations in the coating, and polarization is 20 minutes in 25 ℃ silicone oil, and polarized electric field is 1kV/mm.The potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics constant d that adopts this method to obtain
33Be 182pC/N, plane coupling electromechanical coefficient k
pBe 0.48, quality factor q
mBe 686, thickness electromechanical coupling coefficient k
tBe 0.59.Fig. 2 has provided the scanning electron microscope picture of bismuth potassium titanate sodium potassium-sodium niobate pottery.
Claims (2)
1. a potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics is characterized in that its chemical constitution general formula is: (1-x) K
0.5Na
0.5NbO
3-xBi
0.5(K
0.82Na
0.18) TiO
3, wherein: 0＜x＜0.2, x is a molar fraction.
2. the preparation method of potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics as claimed in claim 1 is characterized in that concrete steps are:
(1), be (1-x) K by stoichiometric ratio with salt of wormwood, yellow soda ash, titanium dioxide, bismuthous oxide bismuth trioxide, Niobium Pentxoxide
0.5Na
0.5NbO
3-xBi
0.5(K
0.82Na
0.18) TiO
3Batching, wherein: 0＜x＜0.2;
(2) material that step (1) is prepared is put into the ball mill batch mixing, and ball/material mass ratio is 2～20, and the material of ball is a kind of in iron ball, agate ball, zirconia ball and the alumina balls, and the time of ball milling is 6～14 hours, and rotating speed is 200～450 rev/mins;
(3) the material briquetting that step (2) is mixed, pre-burning is 1～3 hour under 900～1300 ℃ of temperature, and take out the incinerating material and grind, ball milling once more, ball milling time and synchronization rapid (2), powder is crossed 40 mesh sieves then, and the material of ball and ball/material are than same step (2);
(4) powder that step (3) is obtained adds the pure water of its mass ratio 10-45%, the polyacrylic acid ammonia dispersion agent of mass ratio 0.2～2% and the poly (vinyl alcohol) binder of mass ratio 0.2～2%, mixed in 1～3 hour through ball milling and to form slip, ball milling speed is 50～300 rev/mins, adopt the air-stream spraying granulation, obtain particle diameter and be 0.01～1 millimeter potassium-sodium niobate-sodium potassium bismuth titanate powder granule;
(5) powder granule that step (4) is made is put into press, suppresses disk or square sheet under the pressure of 200～900MPa;
(6) disk of step (5) moulding or square sheet are put into 120 ℃ of bakings of baking oven and became plain sheet in 1～6 hour, the plain sheet that to dry is then put into the stove binder removal, temperature rise rate is 30～90 ℃/h at 25～500 ℃ of temperature sections, 500～800 ℃ of temperature sections are 90～120 ℃/h, and be incubated 1～4 hour, furnace cooling at 270 ℃, 360 ℃, 500 ℃ and 800 ℃ respectively;
(7) the plain sheet that step (6) is obtained is put into sintering oven, rises to 1100～1500 ℃ with 2～12 ℃/minute temperature rise rates, is incubated 1～8 hour, and furnace cooling makes potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics then.
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| CN102173766A (en) * | 2011-01-11 | 2011-09-07 | 桂林理工大学 | Bismuth ferrite-sodium bismuth ferrite niobate multiferroic ceramic and preparation method thereof |
| CN102775142A (en) * | 2012-07-19 | 2012-11-14 | 同济大学 | Lead-free electrostrictive ceramic material and preparation method thereof |
| CN102910907A (en) * | 2012-10-22 | 2013-02-06 | 天津大学 | Potassium-sodium niobate-based leadless piezoelectric ceramic and two-step sintering preparation method thereof |
| CN104129987A (en) * | 2014-07-22 | 2014-11-05 | 桂林电子科技大学 | High-temperature leadless nanometer piezoelectric ceramic and preparation method thereof |
| CN104446447A (en) * | 2014-11-09 | 2015-03-25 | 桂林理工大学 | Large-strain lead-free piezoelectric ceramic complex and preparation method thereof |
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| CN101514103A (en) * | 2009-04-03 | 2009-08-26 | 西北工业大学 | Method for preparing potassium-sodium niobate-sodium bismuth titanate nano ceramics |
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| CN102173766A (en) * | 2011-01-11 | 2011-09-07 | 桂林理工大学 | Bismuth ferrite-sodium bismuth ferrite niobate multiferroic ceramic and preparation method thereof |
| CN102775142A (en) * | 2012-07-19 | 2012-11-14 | 同济大学 | Lead-free electrostrictive ceramic material and preparation method thereof |
| CN102775142B (en) * | 2012-07-19 | 2014-04-02 | 同济大学 | Lead-free electrostrictive ceramic material and preparation method thereof |
| CN102910907A (en) * | 2012-10-22 | 2013-02-06 | 天津大学 | Potassium-sodium niobate-based leadless piezoelectric ceramic and two-step sintering preparation method thereof |
| CN104129987B (en) * | 2014-07-22 | 2016-04-06 | 桂林电子科技大学 | A kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof |
| CN104129987A (en) * | 2014-07-22 | 2014-11-05 | 桂林电子科技大学 | High-temperature leadless nanometer piezoelectric ceramic and preparation method thereof |
| CN104446447A (en) * | 2014-11-09 | 2015-03-25 | 桂林理工大学 | Large-strain lead-free piezoelectric ceramic complex and preparation method thereof |
| CN109206135A (en) * | 2018-09-28 | 2019-01-15 | 华中科技大学 | A kind of thermal sensitive ceramic material and preparation method thereof with high-temperature coefficient |
| CN109206135B (en) * | 2018-09-28 | 2020-05-19 | 华中科技大学 | Thermal sensitive ceramic material with high temperature coefficient and preparation method thereof |
| CN109761604A (en) * | 2019-03-07 | 2019-05-17 | 西安工业大学 | A kind of bismuth-sodium titanate base high-temperature dielectric ceramics and preparation method thereof |
| CN109721352A (en) * | 2019-03-16 | 2019-05-07 | 信阳师范学院 | A kind of bismuth-sodium titanate base lead-free piezoelectric ceramic and preparation method thereof using the preparation of microwave material research-on-research station |
| CN109721352B (en) * | 2019-03-16 | 2021-08-20 | 信阳师范学院 | Sodium bismuth titanate-based lead-free piezoelectric ceramic prepared by adopting microwave material scientific workstation 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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Application publication date: 20101124 |