CN106064945A - PZT base piezoelectric ceramic of calcium lithium ytterbium codope and preparation method thereof - Google Patents

PZT base piezoelectric ceramic of calcium lithium ytterbium codope and preparation method thereof Download PDF

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CN106064945A
CN106064945A CN201610390890.0A CN201610390890A CN106064945A CN 106064945 A CN106064945 A CN 106064945A CN 201610390890 A CN201610390890 A CN 201610390890A CN 106064945 A CN106064945 A CN 106064945A
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pzt
piezoelectric ceramic
base piezoelectric
ytterbium codope
pzt base
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刘洪�
张倩
朱建国
余萍
徐威
陈强
肖定全
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Sichuan University
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Abstract

The present invention provides the PZT base piezoelectric ceramic of a kind of calcium, lithium, ytterbium codope, and the chemical general formula of this piezoelectric ceramics is xPb (Ni1/ 3Nb2/3)O3–yPb(Mg1/2W1/2)O3–(1–x–y)Pb(Zr0.5Ti0.5)O3+ u wt%CaCO3+ v wt%Li2CO3+ wmol%Yb2O3, wherein 0.02≤x≤0.15,0.02≤y≤0.15,0.08≤u≤0.5,0.08≤v≤0.5,0≤w≤0.4.Present invention also offers the preparation method of the PZT base piezoelectric ceramic of above-mentioned calcium, lithium, ytterbium codope.This piezoelectric ceramics sintering temperature is low, and has good piezoelectric property and higher Curie temperature concurrently.

Description

PZT base piezoelectric ceramic of calcium lithium ytterbium codope and preparation method thereof
Technical field
The invention belongs to piezoceramic material field, be specifically related to a kind of calcium lithium ytterbium codope PZT base piezoelectric ceramic and Its preparation method.
Background technology
PZT is traditional piezoelectric ceramics, has the effects such as good dielectric, ferroelectricity, piezoelectricity, pyroelectricity, its cost of material Cheap, be suitable to factorial praluction, its doping vario-property can obtain being applicable to the ceramic material of multiple use.Multilayer piezoelectric ceramic There are alternately ceramic layer and interior metal electrode layer.Along with the high speed development of science and technology, multilayer piezoelectric ceramic has obtained increasingly Study widely, be widely used in brake, transducer, sensor.The general interior electricity that Ag-Pd electrode is used for multi-layer ceramics Pole, its co-fired temperature scope is 920～980 DEG C, and the interior electrode of pure Ag is the most less demanding in the sintering temperature of 900 DEG C.
Tradition sinters under about 1200 DEG C of high temperature containing lead piezoelectric ceramics, and internal electrode is or not the purest Ag (fusing point ≈ 961 DEG C) Can use at such high temperatures, and Ag-Pd electrode layer also can be diffused into ceramic layer, cause the deterioration of pottery electric property, Thus affect the reliability of multilayer device.Low temperature co-fired with the 900 of fine silver electrode DEG C, both at home and abroad to how to reduce in order to realize The sintering temperature of PZT base pottery is studied.Research shows, can reduce sintering temperature by adding flux.By ZnO, Na2CO3、CaCO3、Li2CO3、Bi2O3The sintering that can realize under 900 DEG C of low temperature in piezoelectric ceramics is added to CuO.Such as Chan- Hee Nam discloses in American Ceramics (2011,94 (10), 3,442 3448) and adds in PNN PZT 1.0mol%CuO is as flux, it is thus achieved that d33=620pC/N, TCThe piezoelectric ceramics of=200 DEG C.Although the pressure of ceramic material Electrical property is higher, but Curie temperature is relatively low, the most difficult satisfied higher temperature requirements.Han, H.S exist Trans.Electr.Electron.Mater. (2011,12 (6), 249 252) report with 0.1wt%Li2CO3As fluxing Agent joins in PMN PFN PZT system, obtains d33=425pC/N, TCThe piezoelectric ceramics of=351 DEG C.Its Tc is higher, but pressure Electrical property is decreased obviously.
Summary of the invention
Present invention aims to the deficiencies in the prior art, first purpose of the present invention be to provide a kind of calcium, lithium, The PZT base piezoelectric ceramic of ytterbium codope, this piezoelectric ceramics sintering temperature is low, and has good piezoelectric property and higher residence concurrently In temperature；Second object of the present invention is to provide the preparation method of the PZT base piezoelectric ceramic of above-mentioned calcium, lithium, ytterbium codope, with Reduce the sintering temperature of PZT base piezoelectric ceramic, improve piezoelectric property and Curie temperature simultaneously.
For first goal of the invention of the present invention, the present invention provides the PZT base piezoelectricity pottery of a kind of calcium, lithium, ytterbium codope Porcelain, the chemical general formula of this piezoelectric ceramics is xPb (Ni1/3Nb2/3)O3-yPb(Mg1/2W1/2)O3-(1–x–y)Pb(Zr0.5Ti0.5)O3+ U wt%CaCO3+ v wt%Li2CO3+ w mol%Yb2O3, wherein 0.02≤x≤0.15,0.02≤y≤0.15,0.08≤u≤ 0.5,0.08≤v≤0.5,0≤w≤0.4.U wt%, v wt%, the corresponding component of expression account for the PZT base pressure of calcium lithium ytterbium codope The mass percent of electroceramics；W mol% represents that corresponding component accounts for the PZT base piezoelectric ceramic Mole percent of calcium lithium ytterbium codope Ratio.
For second goal of the invention of the present invention, by mixing calcium, lithium, ytterbium in PZT base piezoelectric ceramic so that mixing Under the effect of miscellaneous element, Li+And Yb3+Enter A or B position, under the sintering temperature of 850～950 DEG C, prepare and have good pressure concurrently The PZT base piezoelectric ceramic of electrical property and higher Curie temperature, concrete technology step is as follows:
(1) preparation of PZT based ceramic powder body: the raw material of each component formula amount determined according to chemical general formula is inserted ball milling Machine ball mill crushing mixes, after mix homogeneously at 750～850 DEG C heat preservation sintering 2～4h, insulation is cooled to room temperature again after terminating Secondary carry out ball mill crushing, obtain PZT based ceramic powder body；
(2) pelletize tabletting: add poly-vinyl alcohol solution in step (1) gained PZT based ceramic powder body and carry out pelletize, then By pelletize gained pellet tabletted, obtain PZT base potsherd；
(3) binder removal sintering: by after step (2) gained PZT base potsherd binder removal at 850～950 DEG C heat preservation sintering 2～ 4h, obtains sintering PZT base piezoelectric ceramic sheet；
(4) polarization: after step (3) gained sintering PZT base piezoelectric ceramic sheet surface-coated silver slurry, at 650～750 DEG C Heat preservation sintering 10～20min, insulation is cooled to room temperature after terminating, then polarizes in silicone oil, obtain calcium lithium ytterbium codope PZT piezoelectric ceramics.
In said method, in step (1), twice ball milling is preferably with dehydrated alcohol as disperse medium, and each component raw material is total Amount is preferably 1:(1.2～2.0 with the consumption mass ratio of dehydrated alcohol).On planetary ball mill with 100～450rmp rotating speed Ball milling 10～24h, is dried after ball milling.Described being dried can be to toast 2～3 hours under heat lamp.
In said method, the concrete technology of gained pellet tabletted is preferably: suppress under the pressure of 10～20MPa Become diameter be about 10～15mm, thickness be about 0.8～1.2mm calcium, lithium, the PZT base piezoelectric ceramic sheet of ytterbium codope.
In said method, described in step (2), the mass concentration of poly-vinyl alcohol solution is preferably 5～10%.
In said method, in step (3), the concrete technology of binder removal is preferably: existed by step (2) gained PZT base potsherd 4～10h it are incubated at 450～550 DEG C.
In said method, the mass concentration of silver slurry described in step (4) is 5～15%.
In said method, step (4) is carried out in silicone oil polarize specifically comprises the processes of: in the silicone oil of 80～120 DEG C, Polarization field strength is holding electric field intensity 15～30min under the conditions of 2～5kV/mm.
Compared with prior art, the method have the advantages that
1, the present invention provides calcium, lithium, ytterbium codope PZT base piezoelectric ceramic, sintering temperature is low, is 850～950 DEG C and has Having good piezoelectric property, d33 is up to 565pC/N, at room temperature utilizes Agilent 4294A precise impedance instrument in the frequency of 1kHz Under record dielectric loss and be not more than 3/1000ths, and Curie temperature is more than 290 DEG C.
2, the calcium of present invention offer, lithium, ytterbium codope PZT base piezoelectric ceramic, its thing is pure perovskite phase mutually, such as Fig. 1 institute Show, mix calcium, lithium, ytterbium codope improve sintering activity makes crystal grain dense uniform and growth fully, fine and close, as shown in Figure 2.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the piezoceramic material that embodiment 1～4 prepares.
Scanning electron microscope (SEM) photo of the piezoceramic material that Fig. 2 prepares for embodiment 2.
Fig. 3 is the piezoelectric property figure of the piezoceramic material that embodiment 1～4 prepares.
Fig. 4 is the change of the dielectric constant with temperature of the piezoceramic material that embodiment 1～4 prepares.
Detailed description of the invention
Below by detailed description of the invention, the PZT base piezoelectric ceramic of calcium of the present invention, lithium, ytterbium codope is made further Explanation.
Embodiment 1
(1) preparation of PZT based ceramic powder body
According to formula 0.08Pb (Ni1/3Nb2/3)O3-0.02Pb(Mg1/2W1/2)O3-0.90Pb(Zr0.5Ti0.5)O3+ 0.30wt%CaCO3+ 0.20wt%Li2CO3+ 0mol%Yb2O3Represent, (x=0.08, y=0.02, u=0.30, v=0.20, w =0) calculate each raw material of weighing, with dehydrated alcohol as disperse medium, be 1 according to the mass ratio of each raw material total amount Yu dehydrated alcohol: Each raw material and dehydrated alcohol are added in ball grinder, with the rotating speed ball milling 24h of 100rmp on planetary ball mill, after ball milling by 1.5 Under heat lamp, baking is dried and obtains mixed powder for 2 hours, gained mixed powder is incubated at 800 DEG C 3h, after insulation terminates Being cooled to room temperature and carry out second time ball milling again according to same procedure, after ball milling, under heat lamp, baking is dried for 3 hours, obtains PZT based ceramic powder body；
(2) pelletize tabletting
In step (1) gained PZT based ceramic powder body, add the poly-vinyl alcohol solution that mass concentration is 10wt% make Grain, is then pressed into diameter under the pressure of 10MPa and is about 10mm, and thickness is about the PZT base piezoelectric ceramic disk of 1.2mm；
(3) binder removal sintering
Step (2) gained PZT base potsherd is incubated at 550 DEG C after 4h carries out binder removal, heat preservation sintering at 850 DEG C 4h, obtains sintering PZT base piezoelectric ceramic sheet；
(4) polarization
After the silver slurry of step (3) gained sintering PZT base piezoelectric ceramic disk surfaces coating 10wt%, protect at 650 DEG C Temperature sintering 20min, insulation is cooled to room temperature after terminating, then in the silicone oil of 90 DEG C, under the conditions of Polarization field strength is 5kV/mm Keep electric field intensity 15min to polarize, obtain the PZT piezoelectric ceramics of calcium, lithium, ytterbium codope.
Prepare calcium, lithium, ytterbium codope PZT piezoelectric ceramics XRD figure spectrum see that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is Pure perovskite phase；Use ZJ-3 type quasistatic d33Instrument, the piezoelectric coefficient d recorded33See Fig. 3, for 532pC/N；Utilize Agilent 4980A precise impedance instrument connection temperature controlling stove records the change of dielectric constant with temperature and sees Fig. 4, can obtain the Curie of sample from Fig. 4 Temperature is 307 DEG C.
Embodiment 2
(1) preparation of PZT based ceramic powder body
According to formula 0.08Pb (Ni1/3Nb2/3)O3-0.02Pb(Mg1/2W1/2)O3-0.90Pb(Zr0.5Ti0.5)O3+ 0.30wt%CaCO3+ 0.20wt%Li2CO3+ 0.10mol%Yb2O3Represent, (x=0.08, y=0.02, u=0.30, v= 0.20, w=0.10) each raw material of weighing is calculated, with dehydrated alcohol as disperse medium, according to the matter of each raw material total amount Yu dehydrated alcohol Each raw material and dehydrated alcohol are added in ball grinder for 1:1.5, with the rotating speed ball milling of 450rmp on planetary ball mill by amount ratio 10h, after ball milling, under heat lamp, baking is dried and obtains mixed powder for 3 hours, and gained mixed powder is incubated at 750 DEG C 4h, Insulation is cooled to room temperature and carries out second time ball milling again according to same procedure after terminating, after ball milling, under heat lamp, baking is entered for 3 hours Row is dried, and obtains PZT based ceramic powder body；
(2) pelletize tabletting
In step (1) gained PZT based ceramic powder body, add the poly-vinyl alcohol solution that mass concentration is 8wt% make Grain, is then pressed into diameter under the pressure of 20MPa and is about 14mm, and thickness is about the PZT base piezoelectric ceramic disk of 0.9mm；
(3) binder removal sintering
Step (2) gained PZT base potsherd is incubated at 550 DEG C after 4h carries out binder removal, heat preservation sintering at 900 DEG C 3h, obtains sintering PZT base piezoelectric ceramic sheet；
(4) polarization
After the silver slurry of step (3) gained sintering PZT base piezoelectric ceramic disk surfaces coating 12wt%, protect at 700 DEG C Temperature sintering 10min, insulation is cooled to room temperature after terminating, then in the silicone oil of 120 DEG C, under the conditions of Polarization field strength is 2kV/mm Keep electric field intensity 30min to polarize, obtain the PZT piezoelectric ceramics of calcium, lithium, ytterbium codope.
Prepare calcium, lithium, ytterbium codope PZT piezoelectric ceramics XRD figure spectrum see that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is Pure perovskite phase；Use ZJ-3 type quasistatic d33Instrument, the d of the piezoelectric modulus recorded33See Fig. 3, for 563pC/N；Utilize Agilent 4980A precise impedance instrument connection temperature controlling stove records the change of dielectric constant with temperature and sees Fig. 4, can obtain the Curie of sample from Fig. 4 Temperature is 301 DEG C.SEM figure is as in figure 2 it is shown, SEM shows sample grain shape rule, and crystallization is abundant, dense non-porous hole.
Embodiment 3
(1) preparation of PZT based ceramic powder body
According to formula 0.08Pb (Ni1/3Nb2/3)O3-0.02Pb(Mg1/2W1/2)O3-0.90Pb(Zr0.5Ti0.5)O3+ 0.30wt%CaCO3+ 0.20wt%Li2CO3+ 0.20mol%Yb2O3Represent, (x=0.08, y=0.02, u=0.30, v= 0.20, w=0.20) each raw material of weighing is calculated, with dehydrated alcohol as disperse medium, according to the matter of each raw material total amount Yu dehydrated alcohol Each raw material and dehydrated alcohol are added in ball grinder for 1:1.5, with the rotating speed ball milling of 300rmp on planetary ball mill by amount ratio 18h, after ball milling, under heat lamp, baking is dried and obtains mixed powder for 3 hours, and gained mixed powder is incubated at 850 DEG C 2h, Insulation is cooled to room temperature and carries out second time ball milling again according to same procedure after terminating, after ball milling, under heat lamp, baking is entered for 2 hours Row is dried, and obtains PZT based ceramic powder body；
(2) pelletize tabletting
In step (1) gained PZT based ceramic powder body, add the poly-vinyl alcohol solution that mass concentration is 10wt% make Grain, is then pressed into diameter under the pressure of 15MPa and is about 13mm, and thickness is about the PZT base piezoelectric ceramic disk of 1mm；
(3) binder removal sintering
Step (2) gained PZT base potsherd is incubated at 450 DEG C after 10h carries out binder removal, heat preservation sintering at 950 DEG C 2h, obtains sintering PZT base piezoelectric ceramic sheet；
(4) polarization
After the silver slurry of step (3) gained sintering PZT base piezoelectric ceramic disk surfaces coating 5wt%, it is incubated at 750 DEG C Sintering 10min, insulation is cooled to room temperature after terminating, and then in the silicone oil of 110 DEG C, Polarization field strength is guarantor under the conditions of 4kV/mm Hold electric field intensity 16min to polarize, obtain the PZT piezoelectric ceramics of calcium, lithium, ytterbium codope.
Prepare calcium, lithium, ytterbium codope PZT piezoelectric ceramics XRD figure spectrum see that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is Pure perovskite phase；Use ZJ-3 type quasistatic d33Instrument, the piezoelectric coefficient d recorded33See Fig. 3, for 552pC/N；Utilize Agilent 4980A precise impedance instrument connection temperature controlling stove records the change of dielectric constant with temperature and sees Fig. 4, can obtain the Curie of sample from Fig. 4 Temperature is 300 DEG C.
Embodiment 4
(1) preparation of PZT based ceramic powder body
According to formula 0.08Pb (Ni1/3Nb2/3)O3-0.02Pb(Mg1/2W1/2)O3-0.90Pb(Zr0.5Ti0.5)O3+ 0.30wt%CaCO3+ 0.20wt%Li2CO3+ 0.30mol%Yb2O3Represent, (x=0.08, y=0.02, u=0.30, v= 0.20, w=0.30) each raw material of weighing is calculated, with dehydrated alcohol as disperse medium, according to the matter of each raw material total amount Yu dehydrated alcohol Each raw material and dehydrated alcohol are added in ball grinder for 1:1.5, with the rotating speed ball milling of 200rmp on planetary ball mill by amount ratio 20h, after ball milling, under heat lamp, baking is dried and obtains mixed powder for 3 hours, and gained mixed powder is incubated at 800 DEG C 3h, Insulation is cooled to room temperature and carries out second time ball milling again according to same procedure after terminating, after ball milling, under heat lamp, baking is entered for 3 hours Row is dried, and obtains PZT based ceramic powder body；
(2) pelletize tabletting
In step (1) gained PZT based ceramic powder body, add the poly-vinyl alcohol solution that mass concentration is 10wt% make Grain, is then pressed into diameter under the pressure of 20MPa and is about 15mm, and thickness is about the PZT base piezoelectric ceramic disk of 0.8mm；
(3) binder removal sintering
Step (2) gained PZT base potsherd is incubated at 500 DEG C after 8h carries out binder removal, heat preservation sintering at 900 DEG C 4h, obtains sintering PZT base piezoelectric ceramic sheet；
(4) polarization
After the silver slurry of step (3) gained sintering PZT base piezoelectric ceramic disk surfaces coating 15wt%, protect at 650 DEG C Temperature sintering 15min, insulation is cooled to room temperature after terminating, then in the silicone oil of 80 DEG C, under the conditions of Polarization field strength is 5kV/mm Keep electric field intensity 25min to polarize, obtain the PZT piezoelectric ceramics of calcium, lithium, ytterbium codope.
Prepare calcium, lithium, ytterbium codope PZT piezoelectric ceramics XRD figure spectrum see that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is Pure perovskite phase；Use Chinese Academy of Sciences acoustics ZJ-3 type quasistatic d33Instrument, the piezoelectric coefficient d recorded33See Fig. 3, for 539pC/ N；Fig. 4 is shown in the change utilizing Agilent 4980A precise impedance instrument connection temperature controlling stove to record dielectric constant with temperature, can obtain from Fig. 4 Curie temperature to sample is 304 DEG C.
Embodiment 5
(1) preparation of PZT based ceramic powder body
According to formula 0.08Pb (Ni1/3Nb2/3)O3-0.02Pb(Mg1/2W1/2)O3-0.90Pb(Zr0.5Ti0.5)O3+ 0.30wt%CaCO3+ 0.20wt%Li2CO3+ 0.40mol%Yb2O3Represent, (x=0.08, y=0.02, u=0.30, v= 0.20, w=0.40) each raw material of weighing is calculated, with dehydrated alcohol as disperse medium, according to the matter of each raw material total amount Yu dehydrated alcohol Each raw material and dehydrated alcohol are added in ball grinder for 1:1.5, with the rotating speed ball milling of 400rmp on planetary ball mill by amount ratio 11h, after ball milling, under heat lamp, baking is dried and obtains mixed powder for 2 hours, and gained mixed powder is incubated at 750 DEG C 4h, Insulation is cooled to room temperature and carries out second time ball milling again according to same procedure after terminating, after ball milling, under heat lamp, baking is entered for 3 hours Row is dried, and obtains PZT based ceramic powder body；
(2) pelletize tabletting
In step (1) gained PZT based ceramic powder body, add the poly-vinyl alcohol solution that mass concentration is 6wt% make Grain, is then pressed into diameter under the pressure of 18MPa and is about 10mm, and thickness is about the PZT base piezoelectric ceramic disk of 1.2mm；
(3) binder removal sintering
Step (2) gained PZT base potsherd is incubated at 500 DEG C after 7h carries out binder removal, heat preservation sintering at 900 DEG C 4h, obtains sintering PZT base piezoelectric ceramic sheet；
(4) polarization
After the silver slurry of step (3) gained sintering PZT base piezoelectric ceramic disk surfaces coating 10wt%, protect at 750 DEG C Temperature sintering 12min, insulation is cooled to room temperature after terminating, then in the silicone oil of 120 DEG C, under the conditions of Polarization field strength is 3kV/mm Keep electric field intensity 30min to polarize, obtain the PZT piezoelectric ceramics of calcium, lithium, ytterbium codope.
Prepare calcium, lithium, ytterbium codope PZT piezoelectric ceramics XRD figure spectrum see that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is Pure perovskite phase；Use Chinese Academy of Sciences acoustics ZJ-3 type quasistatic d33Instrument, the d of the piezoelectric modulus recorded33See Fig. 3, for 486pC/N；Utilize Agilent 4980A precise impedance instrument to connect temperature controlling stove to record the change of dielectric constant with temperature and see Fig. 4, can be from It is 307 DEG C that Fig. 4 obtains the Curie temperature of sample.
Embodiment 6
(1) preparation of PZT based ceramic powder body
According to formula 0.02Pb (Ni1/3Nb2/3)O3-0.1Pb(Mg1/2W1/2)O3-0.88Pb(Zr0.5Ti0.5)O3+ 0.10wt%CaCO3+ 0.30wt%Li2CO3+ 0mol%Yb2O3Represent, (x=0.02, y=0.10, u=0.10, v=0.30, w =0) calculate each raw material of weighing, with dehydrated alcohol as disperse medium, be 1 according to the mass ratio of each raw material total amount Yu dehydrated alcohol: Each raw material and dehydrated alcohol are added in ball grinder, with the rotating speed ball milling 24h of 100rmp on planetary ball mill, after ball milling by 1.5 Under heat lamp, baking is dried and obtains mixed powder for 2 hours, gained mixed powder is incubated at 800 DEG C 3h, after insulation terminates Being cooled to room temperature and carry out second time ball milling again according to same procedure, after ball milling, under heat lamp, baking is dried for 3 hours, obtains PZT based ceramic powder body；
(2) pelletize tabletting
In step (1) gained PZT based ceramic powder body, add the poly-vinyl alcohol solution that mass concentration is 10wt% make Grain, is then pressed into diameter under the pressure of 10MPa and is about 10mm, and thickness is about the PZT base piezoelectric ceramic disk of 1.2mm；
(3) binder removal sintering
Step (2) gained PZT base potsherd is incubated at 550 DEG C after 4h carries out binder removal, heat preservation sintering at 850 DEG C 4h, obtains sintering PZT base piezoelectric ceramic sheet；
(4) polarization
After the silver slurry of step (3) gained sintering PZT base piezoelectric ceramic disk surfaces coating 10wt%, protect at 650 DEG C Temperature sintering 20min, insulation is cooled to room temperature after terminating, then in the silicone oil of 90 DEG C, under the conditions of Polarization field strength is 5kV/mm Keep electric field intensity 15min to polarize, obtain the PZT piezoelectric ceramics of calcium, lithium, ytterbium codope.
Embodiment 7
(1) preparation of PZT based ceramic powder body
According to formula 0.15Pb (Ni1/3Nb2/3)O3-0.05Pb(Mg1/2W1/2)O3-0.80Pb(Zr0.5Ti0.5)O3+ 0.08wt%CaCO3+ 0.5wt%Li2CO3+ 0.2mol%Yb2O3Represent, (x=0.15, y=0.05, u=0.08, v=0.5, w =0.2) calculate each raw material of weighing, with dehydrated alcohol as disperse medium, according to the mass ratio of each raw material total amount with dehydrated alcohol be Each raw material and dehydrated alcohol are added in ball grinder by 1:1.5, with the rotating speed ball milling 24h of 100rmp, ball milling on planetary ball mill Under rear heat lamp, baking is dried and obtains mixed powder for 2 hours, and gained mixed powder is incubated at 800 DEG C 3h, and insulation terminates After be cooled to room temperature and again according to same procedure carry out second time ball milling, after ball milling under heat lamp baking within 3 hours, be dried, To PZT based ceramic powder body；
(2) pelletize tabletting
In step (1) gained PZT based ceramic powder body, add the poly-vinyl alcohol solution that mass concentration is 10wt% make Grain, is then pressed into diameter under the pressure of 10MPa and is about 10mm, and thickness is about the PZT base piezoelectric ceramic disk of 1.2mm；
(3) binder removal sintering
Step (2) gained PZT base potsherd is incubated at 550 DEG C after 4h carries out binder removal, heat preservation sintering at 850 DEG C 4h, obtains sintering PZT base piezoelectric ceramic sheet；
(4) polarization
After the silver slurry of step (3) gained sintering PZT base piezoelectric ceramic disk surfaces coating 10wt%, protect at 650 DEG C Temperature sintering 20min, insulation is cooled to room temperature after terminating, then in the silicone oil of 90 DEG C, under the conditions of Polarization field strength is 5kV/mm Keep electric field intensity 15min to polarize, obtain the PZT piezoelectric ceramics of calcium, lithium, ytterbium codope.
Embodiment 8
(1) preparation of PZT based ceramic powder body
According to formula 0.05Pb (Ni1/3Nb2/3)O3-0.15Pb(Mg1/2W1/2)O3-0.80Pb(Zr0.5Ti0.5)O3+ 0.50wt%CaCO3+ 0.09wt%Li2CO3+ 0.2mol%Yb2O3Represent, (x=0.05, y=0.15, u=0.5, v=0.09, W=0.2) calculate each raw material of weighing, with dehydrated alcohol as disperse medium, according to the mass ratio of each raw material total amount with dehydrated alcohol be Each raw material and dehydrated alcohol are added in ball grinder by 1:1.5, with the rotating speed ball milling 24h of 100rmp, ball milling on planetary ball mill Under rear heat lamp, baking is dried and obtains mixed powder for 2 hours, and gained mixed powder is incubated at 800 DEG C 3h, and insulation terminates After be cooled to room temperature and again according to same procedure carry out second time ball milling, after ball milling under heat lamp baking within 3 hours, be dried, To PZT based ceramic powder body；
(2) pelletize tabletting
In step (1) gained PZT based ceramic powder body, add the poly-vinyl alcohol solution that mass concentration is 10wt% make Grain, is then pressed into diameter under the pressure of 10MPa and is about 10mm, and thickness is about the PZT base piezoelectric ceramic disk of 1.2mm；
(3) binder removal sintering
Step (2) gained PZT base potsherd is incubated at 550 DEG C after 4h carries out binder removal, heat preservation sintering at 850 DEG C 4h, obtains sintering PZT base piezoelectric ceramic sheet；
(4) polarization
After the silver slurry of step (3) gained sintering PZT base piezoelectric ceramic disk surfaces coating 10wt%, protect at 650 DEG C Temperature sintering 20min, insulation is cooled to room temperature after terminating, then in the silicone oil of 90 DEG C, under the conditions of Polarization field strength is 5kV/mm Keep electric field intensity 15min to polarize, obtain the PZT piezoelectric ceramics of calcium, lithium, ytterbium codope.
Application examples
The calcium that embodiment 2 prepared, lithium, the PZT based piezoelectric ceramic materials of ytterbium codope are prepared as thickness 0.2 milli Rice, the disk that diameter is 12 millimeters, add that electrode, lead-in wire, diaphragm, shell etc. make electro-acoustic element, prepared electro-acoustic element has Well audio frequency characteristics, illustrates that calcium of the present invention, lithium, the PZT base piezoelectric ceramic of ytterbium codope have good piezoelectric property.

Claims (10)

1. the PZT base piezoelectric ceramic of a calcium lithium ytterbium codope, it is characterised in that the chemical general formula of this piezoelectric ceramics is xPb (Ni1/3Nb2/3)O3-yPb(Mg1/2W1/2)O3-(1–x–y)Pb(Zr0.5Ti0.5)O3+ u wt%CaCO3+ v wt%Li2CO3+w Mol%Yb2O3, wherein 0.02≤x≤0.15,0.02≤y≤0.15,0.08≤u≤0.5,0.08≤v≤0.5,0≤w≤ 0.4；U wt%, v wt% represent that corresponding component accounts for the mass percent of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope；w Mol% represents that corresponding component accounts for the molar percentage of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope.
2. the preparation method of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope described in claim 1, it is characterised in that include following Processing step:
(1) preparation of PZT based ceramic powder body: the raw material of each component formula amount determined according to chemical general formula is inserted ball mill ball Gall broken mixing, after mix homogeneously at 750～850 DEG C heat preservation sintering 2～4h, insulation is cooled to room temperature and again enters after terminating Row ball mill crushing, obtains PZT based ceramic powder body；
(2) pelletize tabletting: add poly-vinyl alcohol solution in step (1) gained PZT based ceramic powder body and carry out pelletize, then will make Grain gained pellet tabletted, obtains PZT base potsherd；
(3) binder removal sintering: by after step (2) gained PZT base potsherd binder removal at 850～950 DEG C heat preservation sintering 2～4h, To sintering PZT base piezoelectric ceramic sheet；
(4) polarization: after step (3) gained sintering PZT base piezoelectric ceramic sheet surface-coated silver slurry, be incubated at 650～750 DEG C Sintering 10～20min, insulation is cooled to room temperature after terminating, then polarizes in silicone oil, obtain the PZT of calcium lithium ytterbium codope Piezoelectric ceramics.
The preparation method of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope the most according to claim 2, it is characterised in that step (1) ball mill crushing described in is with dehydrated alcohol as disperse medium, each component raw material total amount and the consumption quality of dehydrated alcohol Ratio is 1:(1.2～2.0).
The preparation method of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope the most according to claim 3, it is characterised in that described Ball mill crushing is ball mill crushing 10～24h on the planetary ball mill that rotating speed is 100～450rmp, does after ball mill crushing Dry.
The preparation method of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope the most according to claim 4, it is characterised in that described dry Dry is to toast 2～3 hours under heat lamp.
6. according to the preparation side of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope described in any claim in claim 2～5 Method, it is characterised in that described in step (2), pellet is pressed into a diameter of 10～15mm under the pressure of 10～20MPa, thickness is The PZT base piezoelectric ceramic sheet of the calcium lithium ytterbium codope of 0.8～1.2mm.
7. according to the preparation side of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope described in any claim in claim 2～5 Method, it is characterised in that the mass concentration of described poly-vinyl alcohol solution is 5～10%.
8. according to the preparation side of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope described in any claim in claim 2～5 Method, it is characterised in that binder removal described in step (3) is to be incubated 4～10h at 450～550 DEG C.
9. according to the preparation side of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope described in any claim in claim 2～5 Method, it is characterised in that the mass concentration of silver slurry described in step (4) is 5～15%.
10. according to the preparation side of the PZT base piezoelectric ceramic of calcium lithium ytterbium codope described in any claim in claim 2～5 Method, it is characterised in that be polarized in the silicone oil of 80～120 DEG C described in step (4), Polarization field strength is 2～5kV/mm conditions Lower holding electric field intensity 15～30min.
CN201610390890.0A 2016-06-02 2016-06-02 PZT base piezoelectric ceramic of calcium lithium ytterbium codope and preparation method thereof Pending CN106064945A (en)

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CN115466117A (en) * 2021-06-10 2022-12-13 四川大学 Low-temperature prepared PZT-based piezoelectric ceramic with ultrahigh piezoelectric constant

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