CN107089832A - It is a kind of based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate and preparation method thereof - Google Patents
It is a kind of based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate and preparation method thereof Download PDFInfo
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- CN107089832A CN107089832A CN201710405611.8A CN201710405611A CN107089832A CN 107089832 A CN107089832 A CN 107089832A CN 201710405611 A CN201710405611 A CN 201710405611A CN 107089832 A CN107089832 A CN 107089832A
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Abstract
It is Pb (Zn according to molar percentage the invention discloses a kind of based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate and preparation method thereof1/3Nb2/3)x(Ni1/3Nb2/3)y(Zr0.3Ti0.7)1‑x‑yO3+ a Me, wherein Me are quadrivalent element, 0<x<0.1、0.2<y<0.6.Piezoelectric ceramics prepared by the present invention has the high and low loss of dielectric, piezoelectric constant, and performance is stable；And it is simple with preparation technology, cost is low, beneficial to industrialized production, compact structure.Compared with existing niobium zinc, niobium nickel series piezoelectric ceramic, in the ceramics sample prepared by 1180 DEG C.The ceramics of the present invention have higher electric property, low-dielectric loss, and dielectric loss only has 0.65%, and piezoelectric constant reaches that 600pC/N has preferable combination property.The preparation method of the present invention is simple, reliable, cost is low, is easy to industrialized production.
Description
Technical field
The invention belongs to piezoelectric ceramic technology field, more particularly to a kind of piezoelectricity pottery based on niobium zinc, niobium nickel lead zirconate titanate
Porcelain and preparation method thereof.
Background technology
Piezoceramic material is a kind of ceramic material, the function that mechanical energy and electric energy can be mutually changed, this
Performance is referred to as piezoelectric property.Piezoelectric ceramics is in addition to piezoelectric property, also with dielectric properties and mechanical property.Due to piezoelectricity
Ceramic material has these excellent combination properties, along with its preparation technology simply, stably, reliably, is widely used in it
The various aspects of social life, such as in field of electronic materials.Pb(Ni1/3Nb2/3) series piezoelectric ceramic material is since quilt
After Smolenskii and Agranovskaya has found, the concern and research of many researchers have been obtained.Pb(Ni1/3Nb2/3)
O3Belong to complex perovskite structure, meet ABO3Type perovskite structure, the feature with typical Relaxation Ferroelectrics.PNN bases
System has relatively low sintering temperature and higher dielectric constant.The piezoceramic material of PZN bases has higher electricity
Learn performance.On this basis, people have made substantial amounts of research for the piezoceramic material of niobium zinc, niobium nickel system.Cai Xiao peaks et al.
Research finds that niobium zinc, niobium nickel lead zirconate titanate PZN-PNN-PZT piezoceramic materials have preferable electric property, passes through doping
Ca2+、Sr2+、Ba2+The displacement to part Pb or Li Deng element2CO3、Sb2O3Deng entrance PZN-PNN-PZT piezoceramic materials
Inside is obtained compared with dominance energy：Relative dielectric constant εr~7000, piezoelectric strain constant d33=800pC/N, electromechanical coupling factor kp
=0.65.
In summary, prior art is prepared high dielectric and the piezoceramic material of piezoelectric constant；But because PZN-
PNN-PZT formula components are complex, and sintering temperature is interval narrower, causes produced piezoelectric ceramic piece electric property
Stability is relatively low, is unfavorable for industrialized production.
The content of the invention
It is an object of the invention to provide a kind of based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate and preparation method thereof,
Aim to solve the problem that high dielectric and piezoelectric constant ceramic material that prior art prepares, while its dielectric loss is higher, in addition its
Preparation technology is complicated, unstable and cost is high, the problem of being unfavorable for industrialized production.
The present invention is achieved in that a kind of piezoelectric ceramics based on niobium zinc, niobium nickel lead zirconate titanate, it is described based on niobium zinc,
The piezoelectric ceramics of niobium nickel lead zirconate titanate is Pb (Zn according to molar percentage1/3Nb2/3)x(Ni1/3Nb2/3)y(Zr0.3Ti0.7)1-x-yO3+
AMe, wherein Me are quadrivalent element, 0<x<0.1、0.2<y<0.6.
Further, the Me is Ce or Mn；
The Me is Mn.
Further, 0<x<0.04,0.4<y<0.5.
Another object of the present invention is to provide a kind of preparation based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate
Method, the preparation method based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate comprises the following steps：
Step one, raw material is pressed into the mixed in molar ratio, using alcohol and zirconium ball as ball-milling medium ball milling, powder is obtained, by powder
Material is put into baking oven and dried, and crosses 40 mesh sieve；
Step 2, the powder obtained after sieving is put into corundum crucible, is compacted, capping, the pre-burning in chamber type electric resistance furnace
1-3h, then furnace cooling；
Step 3, by pre- burned powder secondary ball milling, drying, sieving, the paraffin for adding 5wt%-7wt% is made
Grain, is sieved afterwards, is then pressed into diameter 12mm, and thickness is 1.2mm ceramic disks；
Step 4, round ceramic piece is put into crucible, sealing, is put into chamber type electric resistance furnace and is sintered, then with stove
Naturally cool to room temperature；
Step 5, the potsherd sintered is cleaned, and is printed silver paste in its upper and lower surface, is placed in stove, is warming up to
800 DEG C and 30min is incubated, naturally cools to room temperature, then burned sample is positioned in silicone oil and is heated to 50-70 DEG C, is applied
Plus 2kV/mm DC electric field, polarize 30min.
Further, raw material is pressed into the mixed in molar ratio, using alcohol and zirconium ball as ball-milling medium ball milling 16h, rotational speed of ball-mill
For 300r/min, powder is obtained, powder is put into 70 DEG C of baking oven and dried, 40 mesh sieve are crossed；
The powder obtained after sieving is put into corundum crucible, is compacted, capping, at 850 DEG C -1000 in chamber type electric resistance furnace
DEG C pre-burning 2h, then furnace cooling.
Further, by pre- burned powder secondary ball milling, drying, sieving, the paraffin for adding 5wt%-7wt% is made
Grain, is sieved afterwards, and diameter 12mm is pressed under 10Mpa pressure, and thickness is 1.2mm ceramic disks；
Round ceramic piece is put into crucible, is sealed, is put into chamber type electric resistance furnace and is sintered, sintering temperature is 1100
DEG C -1300 DEG C, 2h is incubated, then room temperature is naturally cooled to stove；
The potsherd sintered is cleaned, silver paste is printed in its upper and lower surface using screen printing technique, stove is placed in
In, it is warming up to 800 DEG C and is incubated 30min, naturally cool to room temperature, then burned sample is positioned in silicone oil and is heated to
50-70 DEG C, apply 2kV/mm DC electric field, polarize 30min；
The calcined temperature is 850 DEG C；Sintering temperature is 1180 DEG C.
Another object of the present invention is to provide a kind of piezoelectric ceramics system based on niobium zinc, niobium nickel lead zirconate titanate described in
Standby electronic component.
Another object of the present invention is to provide a kind of piezoelectric ceramics system based on niobium zinc, niobium nickel lead zirconate titanate described in
Standby jacquard comb.
Another object of the present invention is to provide a kind of piezoelectric ceramics system based on niobium zinc, niobium nickel lead zirconate titanate described in
Standby piezoelectric filter.
The present invention provide based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate and preparation method thereof, the piezoelectricity of preparation is made pottery
Porcelain has the high and low loss of dielectric, piezoelectric constant, and the characteristics of performance is stable, preparation technology is simple, can be burnt by traditional solid phase
Connection is synthesized, and its sintering range is wider (± 30 DEG C), it is adaptable to high-volume industrial production；It is various in its raw material
Metal oxide Costco Wholesale is relatively low, and can reduce production cost using chemical pure raw material.The pressure prepared through the present invention
Electroceramics has the advantages that high dielectric, piezoelectric constant, low-dielectric loss, compact structure (such as accompanying drawing 2).With existing niobium zinc, niobium nickel
Series piezoelectric ceramic is compared, in the ceramics sample prepared by 1180 DEG C, ceramic higher electric property of the invention, low dielectric
Loss, as shown in table 1, dielectric loss only has 0.65%, and piezoelectric constant reaches that 600pC/N has preferable combination property.This hair
Bright preparation method is simple, reliable, cost is low, is easy to industrialized production.
Brief description of the drawings
Fig. 1 is the preparation method flow provided in an embodiment of the present invention based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate
Figure.
Fig. 2 be doping manganese oxide mass fraction provided in an embodiment of the present invention be respectively 0.0%, 0.2%, 0.4%,
0.6% and 0.8% SEM schematic diagrames.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
It is provided in an embodiment of the present invention based on niobium zinc, niobium nickel lead zirconate titanate piezoelectric ceramics according to molar percentage be Pb
(Zn1/3Nb2/3)x(Ni1/3Nb2/3)y(Zr0.3Ti0.7)1-x-yO3+ a Me, wherein Me are quadrivalent element, 0<x<0.1、0.2<y<0.6.
The Me is Ce or Mn.
The Me is Mn.
Described 0<x<0.04,0.4<y<0.5.
The raw material is Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5And ZnO, MnO2。
As shown in figure 1, the preparation method provided in an embodiment of the present invention based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate
Comprise the following steps：
S101：The raw material is pressed into the mixed in molar ratio, using alcohol and zirconium ball as ball-milling medium ball milling, powder is obtained, will
Powder is put into baking oven and dried, and crosses 40 mesh sieve；
S102：The powder obtained after sieving is put into corundum crucible, is compacted, capping, the pre-burning 1- in chamber type electric resistance furnace
3h, then furnace cooling；
S103:By pre- burned powder secondary ball milling, drying, sieving, the paraffin for adding 5wt%-7wt% is granulated,
Sieved afterwards, be then pressed into diameter 12mm, thickness is 1.2mm ceramic disks；
S104：Round ceramic piece is put into crucible, is sealed, is put into chamber type electric resistance furnace and is sintered, then with stove certainly
So it is cooled to room temperature；
S105：The potsherd sintered is cleaned, silver paste is printed in its upper and lower surface, is placed in stove, is warming up to 800
DEG C and be incubated 30min, naturally cool to room temperature, then burned sample be positioned in silicone oil and is heated to 50-70 DEG C, application
2kV/mm DC electric field, polarize 30min.
The raw material is pressed into the mixed in molar ratio, using alcohol and zirconium ball as ball-milling medium ball milling 16h, rotational speed of ball-mill is
300r/min, obtains powder, and powder is put into 70 DEG C of baking oven and dried, and crosses 40 mesh sieve；
The powder obtained after sieving is put into corundum crucible, is compacted, capping, at 850 DEG C -1000 in chamber type electric resistance furnace
DEG C pre-burning 2h, then furnace cooling；
By pre- burned powder secondary ball milling, drying, sieving, the paraffin for adding 5wt%-7wt% is granulated, and afterwards will
It is sieved, and diameter 12mm is pressed under 10Mpa pressure, and thickness is 1.2mm ceramic disks；
Round ceramic piece is put into crucible, is sealed, is put into chamber type electric resistance furnace and is sintered, sintering temperature is 1100
DEG C -1300 DEG C, 2h is incubated, then room temperature is naturally cooled to stove；
The potsherd sintered is cleaned, silver paste is printed in its upper and lower surface using screen printing technique, stove is placed in
In, it is warming up to 800 DEG C and is incubated 30min, naturally cool to room temperature, then burned sample is positioned in silicone oil and is heated to
50-70 DEG C, apply 2kV/mm DC electric field, polarize 30min.
The calcined temperature is 850 DEG C；Sintering temperature is 1180 DEG C.
The embodiment of the present invention prepare based on niobium zinc, niobium nickel lead zirconate titanate tetravalence adulterate piezoelectric ceramics in electronic component
Application in field.
The application principle of the present invention is further described with reference to specific embodiment.
Embodiment 1：
The piezoelectric ceramics provided in an embodiment of the present invention adulterated based on niobium zinc, niobium nickel lead zirconate titanate tetravalence, it constitutes and rubbed
Your percentage is Pb (Zn1/3Nb2/3)x(Ni1/3Nb2/3)y(Zr0.3Ti0.7)1-x-yO3+ a Me, wherein Me are Mn quadrivalent elements；
The raw material is Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5And ZnO, MnO2。
Formulation parameter：X=0.02, y=0.49, a=0.0%, 0.2%, 0.4%, 0.6% and 0.8%.
The preparation method comprises the following steps：
(1) dispensing
The raw material is pressed into the mixed in molar ratio, using alcohol and zirconium ball as ball-milling medium ball milling 16h, rotational speed of ball-mill is
300r/min, obtains powder, and powder is put into 80 DEG C of baking oven and dried, and crosses 40 mesh sieve；
(2) pre-burning
The powder obtained after step (1) is sieved is put into corundum crucible, is compacted, capping, 900 in chamber type electric resistance furnace
DEG C pre-burning 2h, then furnace cooling；
(3) tabletting
By pre- burned powder secondary ball milling, drying, sieving in step (2), the paraffin for adding 5wt%-7wt% is made
Grain, is sieved afterwards, and diameter 12mm is pressed under 10Mpa pressure, and thickness is 1.2mm ceramic disks；
(4) sinter
The round ceramic piece of step (3) is put into crucible, is sealed, is put into chamber type electric resistance furnace and is sintered, sintering temperature
Spend for 1200 DEG C, be incubated 2h, then naturally cool to room temperature with stove；
(5) silver, polarization are brushed
The potsherd that step (4) is sintered is cleaned, and silver paste is printed in its upper and lower surface using screen printing technique,
It is placed in stove, is warming up to 800 DEG C and is incubated 30min, naturally cool to room temperature, then burned sample is positioned in silicone oil and added
Heat arrives 50-70 DEG C, applies 2kV/mm DC electric field, and polarize 30min.
(6) electric property is tested
Potsherd prepared by potsherd and prior art prepared by the embodiment of the present invention of learning from else's experience, is placed at room temperature, after 24h
Every electric property of sample is measured, and is recorded in table 1.
Table 1 is in the case where 1180 DEG C sinter, the electric parameters of different doping content samples
Wherein piezoelectric constant passes through quasistatic d33Tester method ZJ-3A China, dielectric loss tan δ pass through TH2826-
LCRMeter is measured, using the permittivity ε of precise impedance analyzer (Agilent HP4294A) analysis of materialr, electromechanical coupling
Close coefficient kp, by determining resonant frequency fsWith anti-resonance frequency fp, and calculated according to following formula:
As it can be seen from table 1 the present invention in niobium zinc, niobium nickel lead zirconate-titanate ceramic raw material by adding appropriate tetravalence
MnO2, doping content a=0.4%, and basic components mol ratio x=0.02, y=0.49 are adjusted, from suitable sintering temperature
1180 DEG C prepare piezoelectric ceramics, reduce the niobium zinc, the dielectric loss of niobium nickel series piezoelectric ceramic nearly more than 3 times, the body
The piezoceramic material of system can be widely used in electronic component field, such as jacquard comb, piezoelectric filter etc..
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (9)
1. a kind of piezoelectric ceramics based on niobium zinc, niobium nickel lead zirconate titanate, it is characterised in that described to be based on niobium zinc, niobium nickel zirconium metatitanic acid
The piezoelectric ceramics of lead is Pb (Zn according to molar percentage1/3Nb2/3)x(Ni1/3Nb2/3)y(Zr0.3Ti0.7)1-x-yO3+ aMe, wherein Me
For quadrivalent element, 0<x<0.1、0.2<y<0.6.
2. the piezoelectric ceramics as claimed in claim 1 based on niobium zinc, niobium nickel lead zirconate titanate, it is characterised in that the Me is Ce
Or Mn；
The Me is Mn.
3. the piezoelectric ceramics as claimed in claim 1 based on niobium zinc, niobium nickel lead zirconate titanate, it is characterised in that 0<x<0.04,
0.4<y<0.5。
4. a kind of preparation method based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate as claimed in claim 1, its feature exists
In the preparation method based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate comprises the following steps：
Step one, raw material is pressed into the mixed in molar ratio, using alcohol and zirconium ball as ball-milling medium ball milling, obtains powder, powder is put
Enter in baking oven and dry, cross 40 mesh sieve；
Step 2, the powder obtained after sieving is put into corundum crucible, is compacted, capping, the pre-burning 1-3h in chamber type electric resistance furnace,
Then furnace cooling；
Step 3, by pre- burned powder secondary ball milling, drying, sieving, the paraffin for adding 5wt%-7wt% is granulated, it
Sieved afterwards, be then pressed into diameter 12mm, thickness is 1.2mm ceramic disks；
Step 4, round ceramic piece is put into crucible, sealing, is put into chamber type electric resistance furnace and is sintered, then natural with stove
It is cooled to room temperature；
Step 5, the potsherd sintered is cleaned, and is printed silver paste in its upper and lower surface, is placed in stove, is warming up to 800 DEG C
And 30min is incubated, room temperature is naturally cooled to, then burned sample is positioned in silicone oil and is heated to 50-70 DEG C, applies 2kV/
Mm DC electric field, polarize 30min.
5. the preparation method as claimed in claim 4 based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate, it is characterised in that
Raw material is pressed into the mixed in molar ratio, using alcohol and zirconium ball as ball-milling medium ball milling 16h, rotational speed of ball-mill is 300r/min, obtains powder
Material, powder is put into 70 DEG C of baking oven and dried, and crosses 40 mesh sieve；
The powder obtained after sieving is put into corundum crucible, is compacted, capping, 850 DEG C of -1000 DEG C of pre-burnings in chamber type electric resistance furnace
2h, then furnace cooling.
6. the preparation method as claimed in claim 4 based on niobium zinc, the piezoelectric ceramics of niobium nickel lead zirconate titanate, it is characterised in that
By pre- burned powder secondary ball milling, drying, sieving, the paraffin for adding 5wt%-7wt% is granulated, sieved afterwards,
Diameter 12mm is pressed under 10Mpa pressure, thickness is 1.2mm ceramic disks；
Round ceramic piece is put into crucible, seal, be put into chamber type electric resistance furnace and be sintered, sintering temperature be 1100 DEG C-
1300 DEG C, 2h is incubated, then room temperature is naturally cooled to stove；
The potsherd sintered is cleaned, silver paste is printed in its upper and lower surface using screen printing technique, is placed in stove, is risen
Temperature is to 800 DEG C and is incubated 30min, naturally cools to room temperature, then burned sample is positioned in silicone oil and is heated to 50-70
DEG C, apply 2kV/mm DC electric field, polarize 30min；
The calcined temperature is 850 DEG C；Sintering temperature is 1180 DEG C.
7. electricity prepared by the piezoelectric ceramics based on niobium zinc, niobium nickel lead zirconate titanate described in a kind of any one of utilization claims 1 to 33
Sub- component.
8. merchant prepared by the piezoelectric ceramics based on niobium zinc, niobium nickel lead zirconate titanate described in a kind of any one of utilization claims 1 to 33
Card comb.
9. pressure prepared by the piezoelectric ceramics based on niobium zinc, niobium nickel lead zirconate titanate described in a kind of any one of utilization claims 1 to 33
Electrical filter.
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| CN109336594A (en) * | 2018-10-26 | 2019-02-15 | 贵州振华电子信息产业技术研究有限公司 | Low rate of change of capacitance piezo ceramic element, piezoelectric ceramics and preparation method thereof |
| CN113185289A (en) * | 2021-03-31 | 2021-07-30 | 哈尔滨工业大学 | Lead manganous niobate-lead nickelate-lead zirconate titanate high-voltage electric ferroelectric ceramic with ultralow dielectric loss and preparation method thereof |
| CN114031398A (en) * | 2021-11-18 | 2022-02-11 | 厦门乃尔电子有限公司 | Composite system high-voltage low-loss piezoelectric ceramic and preparation method thereof |
| CN114890789A (en) * | 2022-04-06 | 2022-08-12 | 山东国瓷功能材料股份有限公司 | Co-fired niobium manganese-lead zirconate titanate piezoelectric ceramic matched with silver inner electrode, and preparation method and product thereof |
| CN115710123A (en) * | 2022-11-23 | 2023-02-24 | 西安交通大学 | Lead-free ferroelectric material and preparation method and application thereof |
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| CN109336594A (en) * | 2018-10-26 | 2019-02-15 | 贵州振华电子信息产业技术研究有限公司 | Low rate of change of capacitance piezo ceramic element, piezoelectric ceramics and preparation method thereof |
| CN109336594B (en) * | 2018-10-26 | 2021-10-01 | 贵州振华电子信息产业技术研究有限公司 | Low-capacitance change rate piezoelectric ceramic element, piezoelectric ceramic and manufacturing method thereof |
| CN113185289A (en) * | 2021-03-31 | 2021-07-30 | 哈尔滨工业大学 | Lead manganous niobate-lead nickelate-lead zirconate titanate high-voltage electric ferroelectric ceramic with ultralow dielectric loss and preparation method thereof |
| CN113185289B (en) * | 2021-03-31 | 2022-06-03 | 哈尔滨工业大学 | Lead manganous niobate-lead nickelate-lead zirconate titanate high-voltage electric ferroelectric ceramic with ultralow dielectric loss and preparation method thereof |
| CN114031398A (en) * | 2021-11-18 | 2022-02-11 | 厦门乃尔电子有限公司 | Composite system high-voltage low-loss piezoelectric ceramic and preparation method thereof |
| CN114890789A (en) * | 2022-04-06 | 2022-08-12 | 山东国瓷功能材料股份有限公司 | Co-fired niobium manganese-lead zirconate titanate piezoelectric ceramic matched with silver inner electrode, and preparation method and product thereof |
| CN115710123A (en) * | 2022-11-23 | 2023-02-24 | 西安交通大学 | Lead-free ferroelectric material and preparation method and application thereof |
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Application publication date: 20170825 |