CN104129987B - A kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof - Google Patents

A kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof Download PDF

Info

Publication number
CN104129987B
CN104129987B CN201410350877.3A CN201410350877A CN104129987B CN 104129987 B CN104129987 B CN 104129987B CN 201410350877 A CN201410350877 A CN 201410350877A CN 104129987 B CN104129987 B CN 104129987B
Authority
CN
China
Prior art keywords
tio
igreatt
preparation
piezoelectric ceramics
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201410350877.3A
Other languages
Chinese (zh)
Other versions
CN104129987A (en
Inventor
周昌荣
周秀娟
曾卫东
杨华斌
周沁
陈国华
袁昌来
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guilin University of Electronic Technology
Original Assignee
Guilin University of Electronic Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guilin University of Electronic Technology filed Critical Guilin University of Electronic Technology
Priority to CN201410350877.3A priority Critical patent/CN104129987B/en
Publication of CN104129987A publication Critical patent/CN104129987A/en
Application granted granted Critical
Publication of CN104129987B publication Critical patent/CN104129987B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention discloses a kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof, composition is with Formula B i 1/2na 1/2?tiO 3+ <i></iGreatT.Gre aT.GT<i>x</iGrea tT.GreaT.GT? (30Li 2o-50SiO 2-20Al 2o 3) or Bi 1/2na 1/2?tiO 3+ <i></iGreatT.Gre aT.GT<i>x</iGrea tT.GreaT.GT? (20Bi 2o 3-40SiO 2-40Al 2o 3) or Bi 1/2na 1/2?tiO 3+ <i></iGreatT.Gre aT.GT<i>x</iGrea tT.GreaT.GT? (30B 2o 3-35SiO 2-35Al 2o 3) represent, wherein <i>x</iGreatT.Gr eaT.GT represents molar fraction, 0 & lt; <i>x</iGreatT.Gr eaT.GT & lt; 0.3.The present invention adopts Amorphous Crystallization legal system for nano ceramics technology, namely avoids grain growth, obtains again very high density.Preparation technology of the present invention is simple, stable, is applicable to commercial introduction application.Pottery composition of the present invention is a kind of environmental type piezoelectric ceramics, and high-temperature stability is good, umpolarization temperature <i>T</iGreatT.Gr eaT.GT daMP.AMp.Amp gt; 500 ° of C, loss is low, has good application prospect at high-temperature piezoelectric sensor.

Description

A kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof
Technical field
The present invention relates to piezoceramic material, specifically a kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof.
Background technology
Piezoelectric ceramics is that a kind of power by change is converted to electricity or electricity is converted to the new function stupalith of vibration, is widely used in wave filter, driving mechanism, resonator, sensor, chews among various electronic devices and components such as ring device and ultrasonic transducer etc.Along with the requirement of the miniaturization to electronic devices and components, functionalization, low cost, high stability is higher, certainly will require that piezoelectric has updating decision, technical development is fast, performance good, wide in variety, rise in value high, pollute the advantages such as few.
Nano ceramics because of the electric property of excellence, mechanical property, oxidation-resistance, corrosion-resistant and with superplasticity like metal species, show tempting application prospect.But the preparation of the nano ceramics of high-compactness is but very difficult.Promote that at high temperature sintering in the process of densification, the fast growth of the crystal grain that invariably accompanies, greatly constrains the widespread use of nano ceramics.At present, nanometer piezoelectric ceramics and preparation method thereof also rarely seen report.
Summary of the invention
The object of the invention is to provide high-temp leadless nanometer piezoelectric ceramics and preparation method thereof, this unleaded nano ceramics has excellent piezoelectric property and high-temperature stability, umpolarization temperature t d>500 ° of C, use temperature exceedes its Curie temperature t c, environmental friendliness, loss are low.
The technical scheme realizing the object of the invention is:
A kind of high-temp leadless nanometer piezoelectric ceramics, its formula chemical formula is:
Bi 1/2na 1/2tiO 3+ x(30Li 2o-50SiO 2-20Al 2o 3) or
Bi 1/2na 1/2tiO 3+ x(20Bi 2o 3-40SiO 2-40Al 2o 3) or
Bi 1/2Na 1/2TiO 3+ x(30B 2O 3-35SiO 2-35Al 2O 3)
Wherein xrepresent molar fraction, 0< x<0.3.
The preparation method of high-temp leadless nanometer piezoelectric ceramics of the present invention, comprises the steps:
(1) by raw material according to chemical formula
Bi 1/2na 1/2tiO 3+ x(30Li 2o-50SiO 2-20Al 2o 3) or
Bi 1/2na 1/2tiO 3+ x(20Bi 2o 3-40SiO 2-40Al 2o 3) or
Bi 1/2Na 1/2TiO 3+ x(30B 2O 3-35SiO 2-35Al 2O 3)
Wherein xrepresent molar fraction, 0< x<0.3.
Preparing burden, take dehydrated alcohol as medium ball milling 10 hours, is incubated 0.5 hour forms uniform glass metal after drying in crucible with 1250-1300 ° of C;
(2) fast the glass metal mixed is poured on the copper coin being preheating to 400 ° of C, is pressed into the sheet glass that thickness is about 1.0mm.
(3) sheet glass prepared is warmed up to 400-550 ° of C with the temperature rise rate of 1 ° of C/min and is incubated 5-18 hour forming core, be then warmed up to 650-800 ° of C with the temperature rise rate of 1 ° of C/min and be incubated 48 hours crystallizatioies, take out and cool fast;
(4) sample is processed into the thin slice that two sides is smooth, thickness is about 1mm, drapes over one's shoulders silver electrode, then tests piezoelectric property.
The present invention adopts Amorphous Crystallization legal system for nano ceramics technology, namely avoids grain growth, obtains again very high density.Preparation technology of the present invention is simple, stable, is applicable to commercial introduction application.Pottery composition of the present invention is a kind of environmental type piezoelectric ceramics, and high-temperature stability is good, umpolarization temperature t d>500 ° of C, loss is low, has good application prospect at high-temperature piezoelectric sensor.
Embodiment
Embodiment 1:
Composition is: Bi 1/2na 1/2tiO 3+ x(30Li 2o-50SiO 2-20Al 2o 3), wherein x=0.18.
Preparation method comprises the steps:
With analytical pure Bi 2o 3, Na 2cO 3, Li 2cO 3, SiO 2, Al 2o 3and TiO 2for raw material, according to following chemical formula Bi 1/2na 1/2tiO 3+ x(30Li 2o-50SiO 2-20Al 2o 3) ( x=0.18) preparing burden, take dehydrated alcohol as medium wet-milling 10 hours, dries.
The powder of drying is incubated 0.5 hour in 1280 ° of C in crucible, is then poured into by the glass metal mixed on the copper coin being preheating to 400 ° of C, is pressed into the sheet glass that thickness is about 1.0mm.
The sheet glass prepared is warmed up to 480 ° of C with the temperature rise rate of 1 ° of C/min and is incubated 12 hours, be then warmed up to 750 ° of C with the temperature rise rate of 1 ° of C/min and be incubated 48 hours, take out and cool fast;
Sample is processed into the thin slice that two sides is smooth, thickness is about 1mm, drapes over one's shoulders silver electrode, then tests piezoelectric property.
Performance is as shown in table 1.
Embodiment 2:
Composition is: Bi 1/2na 1/2tiO 3+ x(20Bi 2o 3-40SiO 2-40Al 2o 3), wherein x=0.22.
Preparation method with embodiment 1, unlike, glass melting temperature 1250 ° of C, nucleation temperature 420 ° of C, recrystallization temperature 720 ° of C.
Performance is as shown in table 1.
Embodiment 3:
Composition is: Bi 1/2na 1/2tiO 3+ x(30B 2o 3-35SiO 2-35Al 2o 3), wherein x=0.28.
Preparation method with embodiment 1, unlike, glass melting temperature 1250 ° of C, nucleation temperature 400 ° of C, recrystallization temperature 670 ° of C.
Performance is as shown in table 1.
Embodiment 4:
Composition is: Bi 1/2na 1/2tiO 3+ x(30B 2o 3-35SiO 2-35Al 2o 3), wherein x=0.12.
Preparation method with embodiment 1, unlike, glass melting temperature 1300 ° of C, nucleation temperature 550 ° of C, recrystallization temperature 800 ° of C.
Performance is as shown in table 1.
Embodiment 5:
Composition is: Bi 1/2na 1/2tiO 3+ x(20Bi 2o 3-40SiO 2-40Al 2o 3), wherein x=0.15.
Preparation method with embodiment 1, unlike, glass melting temperature 1260 ° of C, nucleation temperature 535 ° of C, recrystallization temperature 785 ° of C.
Performance is as shown in table 1.
Embodiment 6:
Composition is: Bi 1/2na 1/2tiO 3+ x(20Bi 2o 3-40SiO 2-40Al 2o 3), wherein x=0.08.
Preparation method with embodiment 1, unlike, glass melting temperature 1300 ° of C, nucleation temperature 545 ° of C, recrystallization temperature 795 ° of C.
Performance is as shown in table 1.
Embodiment 7:
Composition is: Bi 1/2na 1/2tiO 3+ x(30Li 2o-50SiO 2-20Al 2o 3), wherein x=0.10.
Unlike, glass melting temperature 1300 ° of C, nucleation temperature 550 ° of C, recrystallization temperature 800 ° of C.
Performance is as shown in table 1.
Embodiment 8:
Composition is: Bi 1/2na 1/2tiO 3+ x(30Li 2o-50SiO 2-20Al 2o 3), wherein x=0.26.
Unlike, glass melting temperature 1250 ° of C, nucleation temperature 510 ° of C, recrystallization temperature 700 ° of C.
Performance is as shown in table 1.
The electrical property of table 1 embodiment sample
Sample d 33(pC/N) T d(°C) Tanδ(%)
Embodiment 1 16 >500 0.3
Embodiment 2 12 >500 0.2
Embodiment 3 7 >500 0.5
Embodiment 4 10 >500 0.3
Embodiment 5 8 >500 0.4
Embodiment 6 9 >500 0.8
Embodiment 7 11 >500 0.6
Embodiment 8 12 >500 0.3
By the embodiment provided, can clearly understand content of the present invention further above, but they not limitation of the invention.

Claims (2)

1. a high-temp leadless nanometer piezoelectric ceramics, is characterized in that: composition general formula is:
Bi 1/2na 1/2tiO 3+ x(30Li 2o-50SiO 2-20Al 2o 3) or
Bi 1/2na 1/2tiO 3+ x(20Bi 2o 3-40SiO 2-40Al 2o 3) or
Bi 1/2Na 1/2TiO 3+ x(30B 2O 3-35SiO 2-35Al 2O 3)
Wherein xrepresent molar fraction, 0< x<0.3.
2. the preparation method of high-temp leadless nanometer piezoelectric ceramics as claimed in claim 1, is characterized in that: comprise the steps:
(1) by raw material according to chemical constitution general formula:
Bi 1/2na 1/2tiO 3+ x(30Li 2o-50SiO 2-20Al 2o 3) or
Bi 1/2na 1/2tiO 3+ x(20Bi 2o 3-40SiO 2-40Al 2o 3) or
Bi 1/2Na 1/2TiO 3+ x(30B 2O 3-35SiO 2-35Al 2O 3)
Wherein xrepresent molar fraction, 0< x<0.3,
Preparing burden, take dehydrated alcohol as medium ball milling 10 hours, is incubated 0.5 hour after drying in crucible with 1250-1300 ° of C;
(2) fast the glass metal mixed is poured on the copper coin being preheating to 400 ° of C, is pressed into the sheet glass that thickness is 1.0mm;
(3) sheet glass prepared is warmed up to 400-550 ° of C with the temperature rise rate of 1 ° of C/min and is incubated 5-18 hour forming core, be then warmed up to 650-800 ° of C with the temperature rise rate of 1 ° of C/min and be incubated 48 hours crystallizatioies, take out and cool fast;
(4) sample is processed into that two sides is smooth, the thin slice of thickness 1mm, drapes over one's shoulders silver electrode, then tests piezoelectric property.
CN201410350877.3A 2014-07-22 2014-07-22 A kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof Active CN104129987B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410350877.3A CN104129987B (en) 2014-07-22 2014-07-22 A kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410350877.3A CN104129987B (en) 2014-07-22 2014-07-22 A kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof

Publications (2)

Publication Number Publication Date
CN104129987A CN104129987A (en) 2014-11-05
CN104129987B true CN104129987B (en) 2016-04-06

Family

ID=51802896

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410350877.3A Active CN104129987B (en) 2014-07-22 2014-07-22 A kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof

Country Status (1)

Country Link
CN (1) CN104129987B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107082632B (en) * 2017-04-25 2019-07-23 成都新柯力化工科技有限公司 A kind of piezoelectric material and preparation method adapting to hot environment
CN116178009B (en) * 2023-03-17 2023-12-15 江苏师范大学 High-orientation potassium-sodium niobate-based transparent piezoelectric ceramic and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101200369A (en) * 2007-07-27 2008-06-18 桂林电子科技大学 Titanium niobic zincic acid bismuth sodium system leadless piezo-electric ceramic and preparation method thereof
CN101215172A (en) * 2008-01-09 2008-07-09 华中科技大学 Method for preparing bismuth sodium titanate base leadless piezoelectricity thick film
CN101217180A (en) * 2008-01-09 2008-07-09 华中科技大学 A preparation method for lead-free piezoelectricity thick film
CN101891474A (en) * 2010-07-08 2010-11-24 桂林理工大学 Potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101200369A (en) * 2007-07-27 2008-06-18 桂林电子科技大学 Titanium niobic zincic acid bismuth sodium system leadless piezo-electric ceramic and preparation method thereof
CN101215172A (en) * 2008-01-09 2008-07-09 华中科技大学 Method for preparing bismuth sodium titanate base leadless piezoelectricity thick film
CN101217180A (en) * 2008-01-09 2008-07-09 华中科技大学 A preparation method for lead-free piezoelectricity thick film
CN101891474A (en) * 2010-07-08 2010-11-24 桂林理工大学 Potassium-sodium niobate-sodium potassium bismuth titanate piezoelectric ceramics and preparation method thereof

Also Published As

Publication number Publication date
CN104129987A (en) 2014-11-05

Similar Documents

Publication Publication Date Title
George et al. Synthesis and microwave dielectric properties of novel temperature stable high Q, Li2ATi3O8 (A= Mg, Zn) ceramics
CN110272270B (en) Bismuth ferrite-barium titanate-based high-temperature lead-free piezoelectric ceramic with low dielectric loss and high-temperature stability and preparation method thereof
CN102260044B (en) Energy storage niobate microcrystalline glass dielectric material and preparation method thereof
CN102584195B (en) Bismuth-based perovskite type leadless piezoelectric ceramic and low-temperature preparation method thereof
CN102531638B (en) Additive and application thereof for reducing sintering temperature of piezoceramic
Babu et al. Structural, thermal and dielectric properties of lithium zinc silicate ceramic powders by sol-gel method
Zhang et al. Novel low‐firing forsterite‐based microwave dielectric for LTCC applications
Zhang et al. Microwave dielectric properties of CaWO4–Li2TiO3 ceramics added with LBSCA glass for LTCC applications
Chen et al. Silver co‐firable Li2ZnTi3O8 microwave dielectric ceramics with LZB glass additive and TiO2 dopant
CN103030390B (en) Zinc oxide piezoresistor material and preparation method
Anjana et al. Microwave dielectric properties and low‐temperature sintering of cerium oxide for LTCC applications
CN104402425B (en) A kind of preparation method of low-loss bismuth ferrite-barium titanate base piezoelectric ceramic
CN103833354B (en) A kind of solid solution modification metatitanic acid bismuth sodium system leadless piezo-electric ceramic and preparation method thereof
CN102775069A (en) Preparation method of barium strontium titanate based glass ceramic energy storage material
CN104129987B (en) A kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof
CN102199036A (en) Method for preparing energy storage ceramic with high breakdown strength
CN107151138B (en) Low-loss ultrahigh-voltage-performance lead-free piezoelectric ceramic material and preparation method thereof
CN102320828B (en) Unleaded piezoelectric ceramic consisting of B-site composite Bi-based compound and preparation method thereof
CN106187189B (en) A kind of energy storage microwave dielectric ceramic materials and preparation method thereof
CN103922725A (en) Low temperature sintering temperature-stable microwave dielectric ceramic material and preparation method thereof
CN103524127B (en) High-frequency grain boundary layer ceramic capacitor medium and preparation method
CN111217604B (en) Preparation method of sodium bismuth titanate-based electronic ceramic with high energy storage density and efficiency
CN103090661B (en) Piezoelectric ceramic blank piece sintering device and craft method thereof
CN107903055A (en) A kind of grade doping bismuth-sodium titanate Quito layer leadless piezoelectric ceramics
Abhilash et al. Facile synthesis of “Quench‐Free Glass” and ceramic‐glass composite for LTCC applications

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant