CN101423391B - Novel potassium niobate sodium base leadless piezoelectric ceramics and preparation method thereof - Google Patents

Novel potassium niobate sodium base leadless piezoelectric ceramics and preparation method thereof Download PDF

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Publication number
CN101423391B
CN101423391B CN2008100739060A CN200810073906A CN101423391B CN 101423391 B CN101423391 B CN 101423391B CN 2008100739060 A CN2008100739060 A CN 2008100739060A CN 200810073906 A CN200810073906 A CN 200810073906A CN 101423391 B CN101423391 B CN 101423391B
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sintering
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CN101423391A (en
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刘心宇
江民红
陈国华
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Guilin University of Electronic Technology
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Guilin University of Electronic Technology
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Abstract

The invention discloses a potassium-sodium niobate based lead-free piezoelectric ceramic and a method for preparing the same. The novel potassium-sodium niobate based lead-free piezoelectric ceramic is mainly characterized by taking Na2CO3, K2CO3, Nb2O5, Li2CO3, Sb2O3, Bi2O3 and Fe2O3 as raw materials through the traditional potting process according to a chemical formula of (1-x-y)(K0.5Na0.5)NbO3-xLiSbO3-yBiFeO3 to prepare a new ceramic product, wherein x is more than or equal to 0 and less than or equal to 0.1 and y is more than or equal to 0 and less than or equal to 0.05 for mixing materials. By selecting the appropriate x and y values and the appropriate process parameter, the piezoelectric constant d33 of the system can reach more than 250 pC/N, the planar electromechanical coupling factor kp can reach more than 0.51, the Curie temperature is more than 365 DEG C, the dielectric loss (tan theta) at a temperature of below 200 DEG C is less than 3 percent, the dielectric loss (tan theta) at a temperature of below 400 DEG C is less than 7 percent, and the sintering temperature is below 1,130 DEG C.

Description

A kind of potassium niobate sodium-based leadless piezoelectric ceramic and preparation method thereof
Technical field
The present invention relates to lead-free piezoceramic material, specifically is K 0.5Na 0.5NbO 3-LiSbO 3-BiFeO 3Series lead-free piezoelectric ceramic and preparation method thereof.
Background technology
Potassium-sodium niobate (K 0.5Na 0.5NbO 3, be called for short KNN) and be the ferroelectrics of a kind of A position complex perovskite structure, its Curie temperature height (＞300 ℃), the good (d of piezoelectric property 33Can surpass 100pC/N), specific inductivity is low, and density is little, and frequency constant is big, is beneficial to frequency applications, and particularly the application in ultrasonic field is considered to one of candidate material of current leadless piezoelectric ceramics.Yet, volatile under Na and the K high temperature, adopt traditional ceramics technology to be difficult to obtain the good ceramic body of compactness, adopt hot pressing or isostatic pressing process can obtain fine and close KNN pottery, the temperature stability of material is greatly improved, and relative density can reach 99%, but the extent of stability of material does not make us very satisfied, and the heat pressing process production cost is higher, and the scantling size is restricted.
In recent years, people have carried out various study on the modification to potassium niobate sodium-based leadless piezoelectric ceramic, for example solid solution modification, doping vario-property, process modification etc.But the over-all properties of the material that is obtained is still undesirable, or the piezoelectric property of material is good but the technology cost is too high, and perhaps the loss of material is bigger, and perhaps the Curie temperature of material is low excessively; The technology cost is low, but piezoelectric property does not reach application requiring again, and perhaps the density of material is low; Or the like.
Summary of the invention
The purpose of this invention is to provide a kind ofly adopt the dielectric loss of traditional ceramics sintering process preparation low, the potassium niobate sodium-based leadless piezoelectric ceramic of Curie temperature and density height, piezoelectric property excellence and preparation method thereof.
The object of the invention realizes by following technical proposals: at K 0.5Na 0.5NbO 3-LiSbO 3The middle BiFeO that adds 3The leadless piezoelectric ceramics that constitutes can be used general formula (1-x-y) (K 0.5Na 0.5) NbO 3-x LiSbO 3-yBiFeO 3Represent that x, y represent molar content in the ceramic systems in the formula, wherein 0≤x≤0.1,0≤y≤0.05.
Its preparation method comprises wet-milling, dries, burns till, secondary ball milling, granulation, compression moulding, sintering, polishes, drapes over one's shoulders in silver, the silicone oil and polarize.When sintering with the heat-up rate to 500 of 60 ℃/h ℃ insulation 2h, again with the heat-up rate to 800 of 120 ℃/h ℃, again with heat-up rate to 1060～1130 ℃ insulation 1～3h sintering of 60 ℃/h.Behind the sintering,, cool to room temperature again with the furnace with the rate of cooling to 800 of 120 ℃/h ℃.
Advantage of the present invention is: potassium niobate sodium-based leadless piezoelectric ceramic has good piezoelectric property and over-all properties.By selecting suitable x, y value and processing parameter, can make the piezoelectric constant d of this system 33Reach more than the 250pC/N planar electromechanical coupling factor k pCan reach more than 0.51, Curie temperature is more than 365 ℃, and dielectric loss below 200 ℃ (tan θ) is lower than dielectric loss below 3%, 400 ℃ (tan θ) and is lower than 7%, and sintering temperature is below 1130 ℃.
Embodiment
Embodiment 1:
With Na 2CO 3, K 2CO 3, Nb 2O 5, Li 2CO 3, Sb 2O 3, Bi 2O 3And Fe 2O 3Be raw material, according to chemical formula: 0.9462 (K 0.5Na 0.5) NbO 3-0.0498LiSbO 3-0.004BiFeO 3
Prepare burden, during sintering with the heat-up rate to 500 of 60 ℃/h ℃ insulation 2h, again with the heat-up rate to 800 of 120 ℃/h ℃, again with heat-up rate to 1060～1130 ℃ insulation 1～3h sintering of 60 ℃/h, with the rate of cooling to 800 of 120 ℃/h ℃, cool to room temperature again with the furnace and form afterwards.Ceramic plate behind the sintering by silver,, polarizes in 80～90 ℃ of silicone oil after 0.5 hour at 630 ℃ of silver ink firings after two-sided parallel polishing, and polarized electric field is 3～4kV/mm, and the polarization time is 15min; Recording performance after static 24 hours is:
d 33(pC/N) Q m k p ε r tanδ(％) ρ(g/m 3)
259 44.48 0.515 1561 2.00 4.51
Embodiment 2:
The preparation method is with embodiment 1, composition expression formula: 0.95 (K 0.5Na 0.5) NbO 3-0.05LiSbO 3-0BiFeO 3
Performance:
d 33(pC/N) Q m k p ε r tanδ(％) ρ(g/m 3)
202 48.25 0.476 1257 3.00 4.47
Embodiment 3:
The preparation method is with embodiment 1, composition expression formula: 0.9443 (K 0.5Na 0.5) NbO 3-0.0497LiSbO 3-0.006BiFeO 3
Performance:
d 33(pC/N) Q m k p ε r tanδ(％) ρ(g/m 3)
193 68.96 0.395 1173 2.30 4.37
Embodiment 4:
The preparation method is with embodiment 1, composition expression formula: 0.9424 (K 0.5Na 0.5) NbO 3-0.0496LiSbO 3-0.008BiFeO 3
Performance:
d 33(pC/N) Q m k p ε r tanδ(％) ρ(g/m 3)
89 39.26 0.200 1124 8.26 4.34
Embodiment 5:
The preparation method is with embodiment 1, composition expression formula: 0.9405 (K 0.5Na 0.5) NbO 3-0.0495LiSbO 3-0.01BiFeO 3
Performance:
d 33(pC/N) Q m k p ε r tanδ(％) ρ(g/m 3)
55 57.19 0.168 1182 12.80 4.29
Embodiment 6:
Be that other is with embodiment 1 1115 ℃ except that sintering temperature among the preparation method, the composition expression formula is with embodiment 5:
0.9405(K 0.5Na 0.5)NbO 3-0.0495LiSbO 3-0.01BiFeO 3
Performance:
d 33(pC/N) Q m k p ε r tanδ(％) ρ(g/m 3)
195 58.70 0.422 1396 2.60 4.54

Claims (1)

1. potassium niobate sodium-based leadless piezoelectric ceramic, it is characterized in that: it is with Na 2CO 3, K 2CO 3, Nb 2O 5, Li 2CO 3, Sb 2O 3, Bi 2O 3And Fe 2O 3Be raw material, according to chemical formula (1-x-y) (K 0.5Na 0.5) NbO 3-xLiSbO 3-yBiFeO 30≤x≤0.1 wherein, prepare burden in 0≤y≤0.05, make through following preparation method: this method comprises batching, wet-milling, dries, burns till, secondary ball milling, granulation, compression moulding, sintering, polishing, by the step that polarizes in silver, the silicone oil, during sintering with the heat-up rate to 500 of 60 ℃/h ℃ insulation 2h, again with the heat-up rate to 800 of 120 ℃/h ℃, again with heat-up rate to 1060～1130 of 60 ℃/h ℃ insulation 1～3h sintering, with the rate of cooling to 800 of 120 ℃/h ℃, cool to room temperature again with the furnace and form behind the sintering.
CN2008100739060A 2008-11-12 2008-11-12 Novel potassium niobate sodium base leadless piezoelectric ceramics and preparation method thereof Expired - Fee Related CN101423391B (en)

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JP5672443B2 (en) * 2010-11-10 2015-02-18 セイコーエプソン株式会社 Liquid ejecting head, liquid ejecting apparatus, piezoelectric element, and method of manufacturing piezoelectric element
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
CN102351535B (en) * 2011-07-15 2014-03-12 桂林电子科技大学 Low-loss sodium potassium niobate-based lead-free piezoelectric ceramic material and preparation method thereof
KR101485284B1 (en) * 2012-06-26 2015-01-21 혼다덴시 가부시키가이샤 Piezoelectric ceramic composition
CN103145417B (en) * 2013-03-20 2014-07-02 桂林电子科技大学 High-property low-cost potassium-sodium niobate base leadless piezoelectric ceramic and preparation method thereof
CN107758742A (en) * 2017-11-13 2018-03-06 桂林电子科技大学 A kind of base metal niobate micro-nano nanowire material and preparation method thereof of lithium, Sb doped
CN115231921B (en) * 2022-07-27 2023-03-31 贵州大学 Ferromagnetic coupling material 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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