CN106220169A - Modified lead nickle niobate lead titanate piezoelectric ceramics and preparation method thereof - Google Patents
Modified lead nickle niobate lead titanate piezoelectric ceramics and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of modified lead nickle niobate lead titanate piezoelectric ceramics, chemical constituent is: Pb1‑xMex(Ni1/3Nb2/3)0.326(ZryTi1‑y)0.674O3+ 3%PbO+3%NiO+zwt%A；Any one or two kinds during Me is strontium and neodymium in formula, A be antimony and yttrium metal-oxide any one.Piezoelectric ceramics of the present invention is by doping strontium and neodymium, antimony or yttrium, form substitution solid solution, obtain the 0.326PNN 0.647PZT piezoelectric ceramics with preferable combination property, this piezoelectric ceramics has the piezoelectricity dielectric properties of excellence, higher Curie temperature and electromechanical coupling factor；Meanwhile, preparation method is simple, and raw material easily obtains, and has industrial applicibility.
Description
Technical field
The present invention relates to field of electronic components manufacturing, be specifically related to a kind of modified lead nickle niobate-lead zirconate titanate piezoelectric pottery
Porcelain and preparation method thereof.
Background technology
Piezoelectric ceramics is a widely used ceramic material of class, because of its stable mechanical property and excellent electrical property
Can, preparation technology is simple, cost is relatively low and is extensively incorporated in the aspects such as sharp light or organisms, military information and aviation.Continue second time
After world war finds barium titanate piezoelectric ceramics, lead zirconate titanate at the beginning of the fifties (PZT) is to be found, and is developed so far piezoelectricity field
Application is exactly at most PZT series piezoelectric ceramic.But, it is common to use piezoelectric be mainly lead zirconates (PZ), lead titanates
(PT) polyploid being composited with relaxation ferroelectrics such as lead magnesio-niobate (PMN), lead zinc niobate (PZN) and lead nickle niobate (PNN)
System, the combination property such as the piezoelectricity of these materials, dielectric, Curie temperature can not meet industrial demand, with traditional pottery
Porcelain preparation technology develops the piezoelectric ceramics of a kind of high comprehensive performance and is just provided with the important actual application value of industry.
PNN-PZT pottery possesses the feature of " flexible material ", such as high piezoelectric modulus, of a relatively high electromechanical coupling
Number, high dielectric constant, low mechanical quality factor etc..Curie temperature and the piezoelectric constant of PZT pottery are higher, and PNN
Dielectric constant is high, but its Curie temperature is but-120 DEG C, being combined by PZT Yu PNN, it is possible to prepare a kind of higher pressure electricity
With the pottery of dielectric properties, Curie temperature is unlikely to again too low simultaneously, meets the requirement of commercial Application.Such as Publication No.
The patent of invention of CN102659404A discloses low-temperature sintering lead nickle niobate-lead titanate piezoelectric ceramics and preparation method thereof, should
Technology discloses raw material Pb3O4, Ni2O3, Nb2O5, ZrO2, TiO2 and CuO, mills by adding water, and is dried, synthesis, tabletting, row
Glue, sintering, obtained by techniques such as galactic poles, but its dielectric properties and piezoelectric property are the best.
At present, the improved method to PNN-PZT system ceramic performance mainly has two kinds: modification by ion-doping and improvement preparation work
Skill.Due to traditional ceramic preparation technology because its technique is simple, low cost, the advantages such as ceramic performance is good of preparation, improve ceramic
The method of performance is mainly modification by ion-doping.In perovskite ABO3 structure, A position and B position ion all can be doped ion and replace
Forming substitution solid solution, the lead ion of Nd ion and Sr ion pair A position substitutes the dielectric properties that can improve pottery, Y-ion and
After the replacement of Sb ion pair B position ion forms solid solution, the piezoelectric property of pottery is greatly improved.To PNN-PZT system pottery
By the ratio of adjustment Zr/Ti near quasi-homotype phase boundary, doping vario-property ion, and find optimum process condition etc. accurately, it is expected to
Obtain the piezoelectric ceramics of comprehensive electrical better performances.
Summary of the invention
In order to be to overcome the deficiencies in the prior art, the present invention provides one to have high tension electricity coefficient, good dielectric constant, relatively
Modified lead nickle niobate-lead titanate piezoelectric ceramics of high electromechanical coupling factor and preparation method thereof.
To achieve these goals, the present invention is achieved through the following technical solutions:
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, chemical constituent is: Pb1-xMex(Ni1/3Nb2/3)0.326
(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A；Any one or two kinds during Me is strontium and neodymium in formula, A be antimony and
The metal-oxide of yttrium any one；0≤x≤0.05 in formula, 0.418≤y≤0.441,0≤z≤1.0.
Preferably, described Me is neodymium, and A is antimony, x=0.015, y=0.433, z=0.75.
The preparation method of a kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, comprises the following steps:
(1) prepared by wet feed: weighs raw material mixing fully according to stoichiometry, adds dehydrated alcohol mixing and ball milling 4-8h,
To wet feed；
(2) pre-burning molding: the wet feed in step (1) is dried, is placed in corundum crucible and adds a cover, at 750-850 DEG C
After temperature lower calcination 1-4h, then use dehydrated alcohol mixing and ball milling 4-8h to obtain secondary wet feed, secondary wet feed is added after drying
After granulating agent pelletize, dry-pressing formed for stock；
(3) sintering polarization: gained stock is placed on corundum plate and after 550 DEG C of insulation 3-5h, stock is put in batch-type furnace
On corundum plate, buried powder obtains porcelain embryo in 1100～1300 DEG C of sintering 1-3h, then by after porcelain indusium silver electrode in 30 DEG C of silicone oil pole
Change processes 5～10 minutes, to obtain final product.
Preferably, described in step (1), raw material is following components: PbO, NiO, Nb2O5、TiO2、ZrO2、Nd2O3、SrCO3、
Y2O3And Sb2O3。
Preferably, the granulating agent described in step (2) is polyvinyl alcohol.
Preferably, the polarizing voltage 1.5～2kV/mm that polarization described in step (3) processes.
The beneficial effects of the present invention is: based on lead nickle niobate-lead zirconate titanate, add neodymium (Nd) in the feed,
Strontium (Sr), the element such as antimony (Sb) and yttrium (Y), use conventional solid synthetic method to carry out synthesizing, sintering, by doping vario-property and technique
Adjustment, formed substitution solid solution, owing to the ionic radius that ionic radius is 0.129nm, Pb2+ of neodymium is 0.119nm.For
The ion that radius is big, after entering solid solution, will occupy the position of lead (A position ion).Simultaneously as neodymium ion price is high, occupy
After lead ion, structure cell arises that the positive charge of surplus.Therefore, in order to keep electric neutrality will produce lead vacancy accordingly,
Lattice also there will be distortion.Now, electric domain wall easy movement.So after neodymium ion doped, the bullet of PNN-PZT piezoceramic material
Property ratio of slenderness and dielectric constant can become big.
In like manner, Sb ion is less due to ionic radius, will occupy the ion position, B position of perovskite structure after entering solid solution
Put.And due to the unstability of Sb3+, in sintering process+the Sb ion of trivalent can transform into the Sb ion of+5 valencys, with height
Valence state carries out replacing the B position ion of+4 valencys, for keeping electric neutrality still can produce lead vacancy, makes ferroelectric domain turn to and becomes easier to,
Thus cause the piezoelectricity dielectric properties of PNN-PZT piezoelectric ceramics to obtain lifting after Sb ion doping.Grain is mixed used by the present invention
Obtaining the 0.326PNN-0.647PZT piezoelectric ceramics with preferable combination property after son, this piezoelectric ceramics has the piezoelectricity of excellence
Dielectric properties, higher Curie temperature and electromechanical coupling factor；Meanwhile, preparation method is simple, and raw material easily obtains, and has industry real
The property used.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of the lead nickle niobate-Lead Zirconate Titanate ceramic material of embodiment 15 preparation；Diffraction in figure
Peak contrasts with standard card, and obtain is the perovskite structure of pure phase, occurs without dephasign.
Fig. 2 is the stereoscan photograph of the lead nickle niobate-Lead Zirconate Titanate ceramic material of embodiment 15 preparation；Crystalline substance in photo
Grain size is from 1 μm to 8 μm, and crystal boundary is high-visible, and porosity is on the low side, and ceramic structure is dense.
Fig. 3 is the dielectric temperature curve of the lead nickle niobate-Lead Zirconate Titanate ceramic material of embodiment 12 preparation.Figure dielectric is normal
The temperature that number peak value is corresponding is 190 DEG C, i.e. Curie temperature.
Detailed description of the invention
The present invention is further described below in conjunction with specific embodiment and accompanying drawing.
Embodiment 1
The preparation method of a kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, comprises the following steps:
(1) dispensing: with commercially available analytical pure PbO, NiO, Nb2O5、TiO2、ZrO2、Nd2O3、SrCO3、Y2O3And Sb2O3For former
Material, stoichiometrically after dispensing, puts in ball grinder and for medium wet grinding with dehydrated alcohol within 4 hours, obtains wet feed and dry；
(2) pre-burning: dried mixed powder in step (1) is placed in alumina crucible, compacting, add a cover, box
Stove calcines 2h in 800 DEG C, repeats wet grinding and once obtain preburning powdered material；
(3) tabletting: after preburning powdered material grinds, then with dehydrated alcohol for solvent wet grinding 8 hours, add after drying
The polyvinyl alcohol (PVA) of 5wt%～10wt% is a granulated into the fine sand grain of mobility, dry-pressing formed under 10～20MPa pressure,
The stock being pressed into is diameter 1 centimetre, the disk of thickness about 1 millimeter；
(4) binder removal: be placed on corundum plate by the disk stock being pressed into and put in batch-type furnace, 550 DEG C are incubated 4 hours, heat up
Speed is 3～6 DEG C/min, carries out organic eliminating；
(5) sintering: being placed on corundum plate by binder removal stock and add lid, bury material with similar powder and bury burning, heating rate is 3
～6 DEG C/min, within 2 hours, obtain porcelain embryo at 1250 DEG C of sintering, naturally cool to room temperature with stove；
(6) polarization: after the porcelain indusium silver electrode that will obtain, polarization processes 5～10 minutes in the silicone oil of 30 DEG C, polarization electricity
Pressure is 1.5～2kV/mm；The piezoelectric ceramic piece polarized carries out piezoelectricity and the survey of mechanical-electric coupling performance according to the standard of IRE
Examination.
Embodiment 2
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, its chemical composition is:
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A；According to embodiment 1
Preparation method, according to different stoichiometries, wherein x=0.005, y=0.426, z=0.
Embodiment 3
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, its chemical composition is:
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A；According to embodiment 1
Preparation method, according to different stoichiometries, wherein x=0.01, y=0.426, z=0.
Embodiment 4
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, its chemical composition is:
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A；According to embodiment 1
Preparation method, according to different stoichiometries, wherein x=0.015, y=0.426, z=0.
Embodiment 5
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, its chemical composition is:
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A；According to embodiment 1
Preparation method, according to different stoichiometries, wherein x=0.02, y=0.426, z=0.
Embodiment 6
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb0.985-xNd0.015Srx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A；According to
The preparation method of embodiment 1, according to different stoichiometries, wherein x=0.00, y=0.426, z=0.
Embodiment 7
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb0.985-xNd0.015Srx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A；According to
The preparation method of embodiment 1, according to different stoichiometries, wherein x=0.01, y=0.426, z=0.
Embodiment 8
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb0.985-xNd0.015Srx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A；According to
The preparation method of embodiment 1, according to different stoichiometries, wherein x=0.03, y=0.426, z=0.
Embodiment 9
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb0.985-xNd0.015Srx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A；According to
The preparation method of embodiment 1, according to different stoichiometries, wherein x=0.05, y=0.426, z=0.
Embodiment 10
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Y2O3, according to embodiment 1
Preparation method, wherein sintering temperature is 1150 DEG C, x=0.015, y=0.426, z=0.
Embodiment 11
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Y2O3, according to embodiment 1
Preparation method, wherein sintering temperature is 1150 DEG C, x=0.015, y=0.426, z=0.1.
Embodiment 12
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Y2O3, according to embodiment 1
Preparation method, wherein sintering temperature is 1150 DEG C, x=0.015, y=0.426, z=0.3.
Embodiment 13
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Y2O3, according to embodiment 1
Preparation method, wherein sintering temperature is 1150 DEG C, x=0.015, y=0.426, z=0.5.
Embodiment 14
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Sb2O3, according to embodiment
The preparation method of 1, wherein sintering temperature is 1300 DEG C, x=0.015, y=0.433, z=0.5.
Embodiment 15
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Sb2O3, according to embodiment
The preparation method of 1, wherein sintering temperature is 1300 DEG C, x=0.015, y=0.433, z=0.75.
Embodiment 16
A kind of modified lead nickle niobate-lead titanate piezoelectric ceramics, consisting of,
Pb1-xNdx(Ni1/3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%Sb2O3, according to embodiment
The preparation method of 1, wherein sintering temperature is 1300 DEG C, x=0.015, y=0.433, z=1.00.
The dielectric of testing example 2-16 and voltage performance, result is as shown in table 1:
Table 1
As can be seen from Table 1, work as x=0.015, when y=0.433, z=0.75, A position doping neodymium, during the doping Sb of B position, burns
Junction temperature is 1300 DEG C, optimal performance: εT 33/ε0=5540, d33=880pC/N, kp=0.65.
Claims (6)
1. modified lead nickle niobate-lead titanate piezoelectric ceramics, it is characterised in that: chemical constituent is: Pb1-xMex(Ni1/ 3Nb2/3)0.326(ZryTi1-y)0.674O3+ 3%PbO+3%NiO+zwt%A；During in formula, Me is strontium and neodymium any one or two
Kind, A be antimony and yttrium metal-oxide any one；0≤x≤0.05 in formula, 0.418≤y≤0.441,0≤z≤1.0.
Modified lead nickle niobate-lead titanate piezoelectric ceramics the most according to claim 1, it is characterised in that: described Me is neodymium,
A is antimony, x=0.015, y=0.433, z=0.75.
3. a preparation method for modified lead nickle niobate-lead titanate piezoelectric ceramics according to claim 1 and 2, it is special
Levy and be: comprise the following steps:
(1) prepared by wet feed: weighs raw material mixing fully according to stoichiometry, adds dehydrated alcohol mixing and ball milling 4-8h, obtain wet
Material；
(2) pre-burning molding: the wet feed in step (1) is dried, is placed in corundum crucible and adds a cover, the temperature of 750-850 DEG C
After lower calcining 1-4h, then use dehydrated alcohol mixing and ball milling 4-8h to obtain secondary wet feed, secondary wet feed is added pelletize after drying
After agent pelletize, dry-pressing formed for stock；
(3) sintering polarization: gained stock is placed on corundum plate and after 550 DEG C of insulation 3-5h, stock is placed in just in batch-type furnace
On beautiful plate, buried powder obtains porcelain embryo in 1100～1300 DEG C of sintering 1-3h, then by after porcelain indusium silver electrode in 30 DEG C of silicone oil at polarization
Manage 5～10 minutes, to obtain final product.
The preparation method of modified lead nickle niobate-lead titanate piezoelectric ceramics the most according to claim 3, it is characterised in that:
Described in step (1), raw material is following components: PbO, NiO, Nb2O5、TiO2、ZrO2、Nd2O3、SrCO3、Y2O3And Sb2O3。
The preparation method of modified lead nickle niobate-lead titanate piezoelectric ceramics the most according to claim 3, it is characterised in that:
Granulating agent described in step (2) is polyvinyl alcohol.
The preparation method of modified lead nickle niobate-lead titanate piezoelectric ceramics the most according to claim 3, it is characterised in that:
The polarizing voltage 1.5～2kV/mm that polarization described in step (3) processes.
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