CN109400153A - It is a kind of to collect the quaternary series ceramic material with high transducing coefficient and preparation applied to piezoelectric energy - Google Patents
It is a kind of to collect the quaternary series ceramic material with high transducing coefficient and preparation applied to piezoelectric energy Download PDFInfo
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Abstract
It is a kind of to collect the quaternary series ceramic material with high transducing coefficient and preparation applied to piezoelectric energy, belong to piezoceramic material field.The basic chemical composition of the ceramic material is (0.2-x) PZN-xPIN-0.8PZT, and x is 0.000~0.100.With ZnO, In2O3、Nb2O5、Pb3O4、ZrO2、TiO2For raw material, using wet-milling, drying, granulation, compression moulding, sintering step.The present invention realizes the miscoordination variation tendency of Effective Regulation piezoelectric charge coefficient and dielectric constant, completely new mentality of designing is provided further to develop high performance piezoelectric energy collecting material, and there is great progradation to the electromechanical transformation performance and industrial applications that piezoelectric energy collecting device is greatly enhanced.
Description
Technical field
The invention belongs to piezoceramic material fields, and in particular to one kind, which is applied to piezoelectric energy, which collects, has high transducing system
Several quaternary system piezoelectric ceramic materials and preparation method.
Background technique
In recent years, wireless sensor network has obtained quick development, especially monitors system, embedded system in environmental Kuznets Curves
System, military security application system and field animal tracking device etc. are widely used.Since wireless sensor passes
The wiring power supply of system or the method cost of replacement battery are excessively high, so how to realize that wireless sensor self-powered is the world today
The hot spot of various countries' research.However the new energy such as solar energy, wind energy are overweight to environmental factor dependence, can not wireless sensor from
Power supply aspect obtains good application.Piezoelectric energy collection technique is to utilize the direct piezoelectric effect of piezoelectric material by the machine in environment
Tool can be converted to electric energy, and have electromechanical high conversion efficiency, output voltage it is high, not by electromagnetic interference, excellent without applied bias etc.
Point, thus have broad application prospects in wireless sensing field.
Currently, being applied to the material of piezoelectric energy collecting device mainly based on piezoelectric monocrystal, but its preparation cost is high, work
Skill is complicated, machinability is poor, thus can not large-scale application.Compared to for the former, Conventional piezoelectric ceramic material has system
It is standby it is at low cost, craftsmanship is simple, the advantages that can be mass-produced, thus the large-scale application that can satisfy collection of energy device needs
It asks.
In order to meet the application request of piezoelectric energy collector, piezoceramic material must have high transducing coefficient
(d33·g33):
d33: piezoelectric charge coefficient g33: piezoelectric field constant
εr: relative dielectric constant ε0: permittivity of vacuum, 8.854 × 10-12F/m by formula (1-1) as can be seen that pair
For piezoceramic material, high transducing coefficient (d33·g33) high piezoelectric charge coefficient (d can be passed through33) and low phase
To dielectric constant (εr) obtain.
So far, the transducing coefficient (d to improve piezoceramic material33·g33), the worker of various countries' related fields into
A large amount of research work is gone, these work mainly include quasi- constructing quasi- homotype phase boundary (MPB), doping and adjusting seed size size
Deng to obtain with high transducing coefficient (d33·g33) piezoceramic material.2013, Zheng etc. was to 0.2Pb (Zn1/ 3Nb2/3)O3-0.8Pb(Zr1/2Ti1/2)O3System has carried out doping vario-property research, the results showed that introducing NiO dopant makes the body
The best transducing coefficient of system has reached 10050 × 10-15m2/N(Journal of the European Ceramic
Society, 2013, volume 33, the 8th phase, 1447-1456 pages).Yue etc. is combined using high-energy ball milling and pressureless sintering technology,
Crystallite dimension is prepared in the other 0.2Pb (Zn of submicron order1/3Nb2/3)O3-0.8Pb(Zr1/2Ti1/2)O3Superfine ceramics, transducing
Coefficient is 7980 × 10-15m2/ N (Journal of the American Ceramic Society, 2017, volume 100,
11 phases, 5211-5219 pages).Piezoelectric charge coefficient (d in above-mentioned former works33) and relative dielectric constant (εr) often table
The variation tendency for revealing while increasing or reducing simultaneously, according to above-mentioned formula (1-1), this collaborative variation, which seriously limits, is changed
It can coefficient (d33·g33) promotion, to be difficult to obtain excellent piezoceramic material to meet high performance piezoelectric collection of energy
The application demand of device.Therefore, it is necessary to seek new design of material thinking significantly to promote the transducing coefficient of piezoceramic material
(d33·g33)。
In conclusion in order to meet the requirement of the high electromechanical transformation performance of piezoelectric energy collecting device, in this patent, mainly
By introducing the constituent element of low relative dielectric constant to the Pb (Zn being widely used at present1/3Nb2/3)O3-Pb(Zr1/2Ti1/2)O3Base (contracting
It is written as PZN-PZT) in ternary system piezoelectric ceramic, to the piezoelectric charge of Effective Regulation PZN-PZT based piezoelectric ceramic materials
Constant (d33) and relative dielectric constant (εr) variation tendency, to greatly improve its transducing coefficient (d33·g33)。
Summary of the invention
The purpose of the present invention is Effective Regulation PZN-PZT base ceramic material piezoelectric charge coefficient (d33) and relative dielectric constant
(εr) variation tendency, to significantly promote the transducing coefficient (d of the material system33·g33).The present invention takes will be low opposite
Pb (the In of dielectric constant1/2Nb1/2)O3(being abbreviated as PIN) relaxation body introduces PZN-PZT ternary system perovskite as compound constituent element
Novel (0.2-x) Pb (Zn is constructed in ferroelectricity matrix1/3Nb2/3)O3-xPb(In1/2Nb1/2)O3-0.8Pb(Zr1/2Ti1/2)O3(contracting
It is written as (0.2-x) PZN-xPIN-0.8PZT) quaternary system piezoelectric ceramic material, to utilize the low opposite dielectric of the compound constituent element of PIN
Constant is greatly lowered the relative dielectric constant (ε of the material systemr), while based on the different electron configurations pair of B cations
The disturbance of random field so that farmland state is optimized, and then stabilizes the piezoelectric charge coefficient (d of the material system33), thus in spy
Fixed composition, which obtains, has high transducing coefficient (d33·g33) quaternary system piezoelectric ceramic material.
To achieve the above object, the present invention takes following technical scheme.
A kind of piezoelectric energy that is applied to provided by the invention is collected with high transducing coefficient (d33·g33) quaternary system piezoelectricity
Ceramic material, which is characterized in that take and introduce PZN-PZT tri- for the relaxation body PIN of low relative dielectric constant as compound constituent element
Member is to construct quaternary system piezoelectric ceramic material in perovskite ferroelectric matrix, the basic chemical composition of the piezoceramic material are as follows:
(0.2-x)Pb(Zn1/3Nb2/3)O3-xPb(In1/2Nb1/2)O3-0.8Pb(Zr1/2Ti1/2)O3(it is abbreviated as (0.2-x) PZN-xPIN-
0.8PZT), wherein the numerical value of x is greater than 0.000 less than 0.100, preferably 0.008-0.075, further preferred 0.042.
The present invention is above-mentioned to have high transducing coefficient (d33·g33) quaternary system piezoelectric ceramic material preparation method, it is special
Sign is, is prepared by conventional solid-state method, specifically includes the following steps:
(1) (0.2-x) PZN-xPIN-0.8PZT ceramic powder is synthesized, weighs raw material according to corresponding chemical mole metering ratio:
ZnO、Nb2O5、Pb3O4、ZrO2、TiO2、In2O3, load weighted raw material is put into ball grinder, is placed in by medium of dehydrated alcohol
Ball milling 24 hours in horizontal ball mill；After ball milling gained slurry dried, then in air atmosphere 850 DEG C calcine 2 hours
Furnace cooling afterwards, then products therefrom (0.2-x) PZN-xPIN-0.8PZT after calcining is subjected to secondary ball milling, gained slurry after ball milling
Material is dried, and (0.2-x) PZN-xPIN-0.8PZT ceramic powder is obtained；
(2) it is granulated using polyvinyl alcohol (PVA) aqueous solution as binder, compression moulding, is bonded in 560 DEG C of exclusions
Then agent is sintered, preferably 1000 DEG C at 950~1150 DEG C, keep the temperature 2 hours, obtain ceramic material.
It is preferred that: the dosage of above-mentioned steps (2) binder is preferably that every 10g ceramic powder corresponds to 1.2ml binder, binder
Mass concentration be 5%.Briquetting pressure is 100MPa.
Sintered potsherd, by polishing treatment later by upper silver electrode, in 120 DEG C of silicone oil, in 40kVcm-1
Voltage under polarize 30min, then aged at room temperature is for 24 hours, and the test of electrical property is then carried out to sample.
Wherein, best sample are as follows: 0.158PZN-0.042PIN-0.8PZT, performance can reach: d33=379pC/N, εr
=1009, d33·g33=16081 × 10-15m2/ N can satisfy the requirement of collection of energy device.
Compared with prior art, the invention has the following beneficial effects:
(1) design method provided by the invention for introducing the low compound constituent element of relative dielectric constant, can effectively solve the problem that piezoelectricity
Charge coefficient (d33) and relative dielectric constant (εr) collaborative variation the problem of, can effectively split piezoelectric charge coefficient (d33) and it is opposite
Dielectric constant (εr) variation tendency, that is, relative dielectric constant (ε is being greatly loweredr) while, maintain piezoelectric charge coefficient
(d33) stabilization, for further develop high performance piezoelectric energy collecting material provide completely new mentality of designing.
(2) of the invention that there is high transducing coefficient (d33·g33) piezoceramic material, energy harvester can be effectively improved
The electromechanical conversion efficiency of part is a kind of potential piezoceramic material applied to collection of energy device.
(3) of the invention that there is high transducing coefficient (d33·g33) piezoceramic material preparation method it is simple, be easy to grasp
Make, at low cost and stable structure, be convenient for industrialized production, there is good industrial applications prospect and significant society and warp
Ji benefit.
Detailed description of the invention
When Fig. 1 is x=0.042 of the invention, i.e. the XRD spectrum of 0.158PZN-0.042PIN-0.8PZT；
Fig. 2 is transmission electron microscope (TEM) figure of (0.2-x) PZN-xPIN-0.8PZT of the invention: (a) x=
0.000, (b) x=0.042；
When Fig. 3 is that present invention group becomes (0.2-x) PZN-xPIN-0.8PZT, x=0.000~0.100, quaternary system piezoelectricity
Piezoelectric ceramics charge coefficient (d33), relative dielectric constant (εr), transducing coefficient (d33·g33) datagram.
Specific embodiment
Below by embodiment the substantive distinguishing features and remarkable advantage that the present invention is furture elucidated.It is noted that the present invention
It is limited only to stated embodiment by no means.
It is provided by the invention that there is high transducing coefficient (d33·g33) quaternary system piezoelectric ceramic material, chemical composition are as follows:
(0.2-x) PZN-xPIN-0.8PZT, wherein the numerical value of x is 0.000~0.100.Piezoceramic material (0.2-x) PZN-
The constitutive material of xPIN-0.8PZT are as follows: Pb3O4、ZnO、Nb2O5、ZrO2、TiO2、In2O3.Specific preparation method is, firstly, synthesis
(0.2-x) PZN-xPIN-0.8PZT ceramic powder weighs raw material according to corresponding chemical metering ratio: ZnO, In2O3、Nb2O5、
Pb3O4、ZrO2、TiO2, load weighted raw material is put into ball grinder, is placed in ball in horizontal ball mill by medium of dehydrated alcohol
Mill 24 hours；After ball milling gained slurry dried, then in air atmosphere 850 DEG C calcining 2 hours after furnace cooling, then will
Products therefrom (0.2-x) PZN-xPIN-0.8PZT carries out secondary ball milling after calcining, and gained slurry is dried after ball milling, obtains
Corresponding ceramic powder.Then use mass concentration for 2%~8% polyvinyl alcohol (PVA) aqueous solution, preferably PVA mass concentration
It is 5%, is granulated as binder, in the forming under the pressure of 100MPa, is pressed into diameter 11.5mm, thickness 1.5mm or so
Molding, in 560 DEG C of exclusion binders, then 950~1150 DEG C be sintered, preferably 1000 DEG C, keep the temperature 2 hours, made pottery
Ceramic material.Sintered potsherd, after polishing treatment, by upper silver electrode, in 120 DEG C of silicone oil, in 40kVcm-1
Voltage under polarize 30min.Then the test of electrical property is carried out to sample, as follows:
(1) dielectric properties are tested
Capacitance C is measured using LCR digital electric bridge (Agilent E4980A), and opposite be situated between is calculated according to formula (1-2)
Electric constant.
In formula
C-capacitance；
T-sample thickness；
A-sample area；
ε0- permittivity of vacuum (8.85 × 10-12F/m)。
(2) piezoelectric property is tested
Using acoustics institute, the Chinese Academy of Sciences quasi-static d of ZJ-2A type33Tester directly reads piezoelectric strain constant d33。
Below by embodiment the substantive distinguishing features and remarkable advantage that the present invention is furture elucidated.It should be appreciated that of the invention
It is limited only to stated embodiment by no means.
Embodiment 1 (i.e. comparative example):
First press matrix chemical formula 0.2Pb (Zn1/3Nb2/3)O3-0.8Pb(Zr1/2Ti1/2)O3(abbreviation 0.2PZN-0.8PZT) claims
Measure Nb2O5、Pb3O4、ZrO2、TiO2And ZnO, and ball milling 24 hours in ethanol.Mixture calcines 2 at 850 DEG C after drying
Hour, 0.2PZN-0.8PZT ceramic powder is obtained after ball milling, drying in ethanol again.0.2PZN-0.8PZT powder is weighed again
Material is mixed in the ratio of 10g powder 1.2mL binder, and the compression moulding object at 100MPa, molding is bonded in 560 DEG C of exclusions
Then agent is sintered, preferably 1000 DEG C at 950~1150 DEG C, be sintered 2 hours, obtains pure 0.2PZN-0.8PZT ceramics.
Embodiment 2:
First press matrix chemical formula 0.192Pb (Zn1/3Nb2/3)O3-0.008Pb(In1/2Nb2/3)O3-0.8Pb(Zr1/2Ti1/2)
O3(abbreviation 0.192PZN-0.008PIN-0.8PZT) weighs Nb2O5、In2O3、Pb3O4、ZrO2、TiO2And ZnO, and in ethanol
Ball milling 24 hours.Mixture is calcined 2 hours at 850 DEG C after drying, is obtained after ball milling, drying in ethanol again
0.192PZN-0.008PIN-0.8PZT ceramic powder.0.192PZN-0.008PIN-0.8PZT powder is weighed again, by 10g powder
The ratio of 1.2mL binder mixes, and the compression moulding object at 100MPa, molding is in 560 DEG C of exclusion binders, then 950
~1150 DEG C of sintering, are sintered 2 hours by preferably 1000 DEG C, obtain 0.192PZN-0.008PIN-0.8PZT ceramics.
Embodiment 3:
By 0.184Pb (Zn1/3Nb2/3)O3-0.016Pb(In1/2Nb2/3)O3-0.8Pb(Zr1/2Ti1/2)O3(abbreviation
0.184PZN-0.016PIN-0.8PZT) form.The other the same as in Example 2.
Embodiment 4:
By 0.175Pb (Zn1/3Nb2/3)O3-0.025Pb(In1/2Nb2/3)O3-0.8Pb(Zr1/2Ti1/2)O3(abbreviation
0.175PZN-0.025PIN-0.8PZT) form.The other the same as in Example 2.
Embodiment 5:
By 0.158Pb (Zn1/3Nb2/3)O3-0.042Pb(In1/2Nb2/3)O3-0.8Pb(Zr1/2Ti1/2)O3(abbreviation
0.158PZN-0.042PIN-0.8PZT) form.The other the same as in Example 2.
Embodiment 6:
By 0.15Pb (Zn1/3Nb2/3)O3-0.05Pb(In1/2Nb2/3)O3-0.8Pb(Zr1/2Ti1/2)O3(abbreviation
0.150PZN-0.05PIN-0.8PZT) form.The other the same as in Example 2.
Embodiment 7:
By 0.125Pb (Zn1/3Nb2/3)O3-0.075Pb(In1/2Nb2/3)O3-0.8Pb(Zr1/2Ti1/2)O3(abbreviation
0.125PZN-0.075PIN-0.8PZT) form.The other the same as in Example 2.
Embodiment 8 (i.e. comparative example):
By 0.1Pb (Zn1/3Nb2/3)O3-0.1Pb(In1/2Nb2/3)O3-0.8Pb(Zr1/2Ti1/2)O3(abbreviation 0.1PZN-
0.1PIN-0.8PZT) form.The other the same as in Example 2.
1 above-described embodiment performance comparison table of table
Claims (7)
1. a kind of collect the quaternary system piezoelectric ceramic material with high transducing coefficient applied to piezoelectric energy, which is characterized in that adopt
It takes the Pb (In of low relative dielectric constant1/2Nb1/2)O3(being abbreviated as PIN) relaxation body introduces PZN-PZT tri- as compound constituent element
Member is that quaternary system piezoelectric ceramic material is constructed in perovskite ferroelectric matrix, the chemical composition of quaternary system piezoelectric ceramic material are as follows:
(0.2-x)Pb(Zn1/3Nb2/3)O3-xPb(In1/2Nb1/2)O3-0.8Pb(Zr1/2Ti1/2)O3, it is abbreviated as (0.2-x) PZN-xPIN-
0.8PZT, wherein the numerical value of x is greater than 0.000 less than 0.100.
2. a kind of four-component-system piezoelectric ceramics collected applied to piezoelectric energy with high transducing coefficient described in accordance with the claim 1
Material, which is characterized in that the numerical value of x is 0.008-0.075.
3. a kind of four-component-system piezoelectric ceramics collected applied to piezoelectric energy with high transducing coefficient described in accordance with the claim 1
Material, which is characterized in that the numerical value of x is 0.042.
4. the method for preparing piezoceramic material described in claim 1, which is characterized in that be prepared by conventional solid-state method
It arrives, specifically includes the following steps:
(1) (0.2-x) PZN-xPIN-0.8PZT ceramic powder is synthesized, weighs raw material according to corresponding chemical mole metering ratio: ZnO,
In2O3、Nb2O5、Pb3O4、ZrO2、TiO2, load weighted raw material is put into ball grinder, is placed in using dehydrated alcohol as medium horizontal
Ball milling 24 hours in ball mill；After ball milling gained slurry dried, then in air atmosphere 850 DEG C calcining 2 hours after with
Furnace is cooling, then will carry out secondary ball milling by products therefrom (0.2-x) PZN-xPIN-0.8PZT after calcining, after ball milling gained slurry into
Row drying, obtains corresponding ceramic powder；
(2) it is granulated using polyvinyl alcohol water solution as binder, then compression moulding excludes binder, then 950
~1150 DEG C of sintering, keep the temperature 2 hours, obtain (0.2-x) PZN-xPIN-0.8PZT ceramic material by preferably 1000 DEG C.
5. according to method for claim 4, which is characterized in that step (2) use mass concentration for 2%~8% polyvinyl alcohol
(PVA) aqueous solution, preferably PVA mass concentration are 5%, are granulated as binder.
6. according to method for claim 4, which is characterized in that step (2) briquetting pressure is 100MPa, is bonded in 560 DEG C of exclusions
Agent.
7. according to method for claim 4, which is characterized in that the dosage of binder is that every 10g ceramic powder corresponds to 1.2ml bonding
Agent.
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