CN106673648A - Ytterbium oxide doped low-temperature prepared PZT (Piezoe-lectric Transducer) based piezoelectric ceramic - Google Patents

Ytterbium oxide doped low-temperature prepared PZT (Piezoe-lectric Transducer) based piezoelectric ceramic Download PDF

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CN106673648A
CN106673648A CN201611176135.9A CN201611176135A CN106673648A CN 106673648 A CN106673648 A CN 106673648A CN 201611176135 A CN201611176135 A CN 201611176135A CN 106673648 A CN106673648 A CN 106673648A
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pzt
ytterbium oxide
piezoelectric ceramic
oxide doped
sintering
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刘洪�
张倩
朱建国
余萍
宋慧瑾
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Sichuan University
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Sichuan University
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Abstract

The invention discloses an ytterbium oxide doped low-temperature prepared PZT (Piezoe-lectric Transducer) based piezoelectric ceramic material and a preparation method thereof. The formula of the piezoelectric ceramic is xPb(Ni1/3Nb2/3))3-yPb(Mg1/2W1/2)O3-(1-x-y)Pb(Zr0.3Ti0.7)O3+u wt% Ba(W1/2Cu1/2)+vmol% Yb2O3, wherein x is great than or equal to 0.1 and less than or equal to 0.8, y is great than or equal to 0.02 and less than or equal to 0.15, u is great than or equal to 0.01 and less than or equal to 0.5, and v is great than or equal to 0 and less than or equal to 0.4. The preparation method comprises the following steps: preparing ytterbium oxide doped PZT based piezoelectric ceramic powder which is sintered at low temperature of 850-950 DEG C by using a solid-phase reaction method, pelleting, tabletting, arranging glue, sintering, performing silver sintering, performing polarization, and the like, thereby obtaining a ceramic material. Results show that the ytterbium oxide doped low-temperature prepared PZT based piezoelectric ceramic material is prepared at the sintering temperature of 850-950 DEG C, the material is dense in crystalline grain, uniform in crystalline grain, sufficient in crystallization and remarkable in liquid-phase sintering characteristic, and the piezoelectric property can be greatly improved.

Description

A kind of ytterbium oxide doping low temperature preparation PZT base piezoelectric ceramic
Technical field
The present invention possess and control in piezoceramic material field, and in particular to a kind of low sintering PZT bases of ytterbium oxide doping Piezoelectric ceramics.
Background technology
PZT is traditional piezoelectric ceramics, with effects such as good dielectric, ferroelectricity, piezoelectricity, pyroelectricities, its cost of material It is cheap, factorial praluction is suitable to, its doping vario-property can be obtained to be applied to the ceramic material of multiple use.Multilayer piezoelectric ceramic There are alternately ceramic layer and interior metal electrode layer.With the high speed development of science and technology, multilayer piezoelectric ceramic has been obtained increasingly Extensive research, is widely used in brake, transducer, sensor.The general interior electricity that Ag-Pd electrodes are used for multi-layer ceramics Pole, its co-fired temperature scope is 920~980 °C, and the interior electrode of pure Ag is then less demanding in 900 °C of sintering temperature.Pass System lead piezoelectric ceramics are sintered under about 1200 °C of high temperature, therefore pure Ag（961 °C of fusing point ≈）Internal electrode can not be so Use at high temperature, and Ag-Pd electrode layers can also be diffused into ceramic layer, cause the deterioration of ceramic electric property, so as to affect The reliability of multilayer device.
The content of the invention
Present invention aims to the deficiencies in the prior art, first purpose of the present invention is to provide a kind of ytterbium oxide The PZT base piezoelectric ceramics of doping, the piezoelectric ceramics sintering temperature is low, and has good piezoelectric property concurrently；The second of the present invention Individual purpose is to provide the preparation method of the PZT base piezoelectric ceramics of above-mentioned ytterbium oxide doping, to reduce the sintering of PZT base piezoelectric ceramics Temperature, while improving piezoelectric property.
For first goal of the invention of the present invention, the present invention provides a kind of PZT base piezoelectric ceramics of ytterbium oxide doping, should The chemical general formula of piezoelectric ceramics isxPb(Ni1/3Nb2/3)O3– yPb(Mg1/2W1/2)O3– (1–x–y)Pb(Zr0.3Ti0.7)O3+uwt% Ba(W1/2Cu1/2)+ v mol% Yb2O3Represent, 0.1≤x≤0.8,0.02≤y≤0.15, 0.01≤ u ≤0.5, 0≤v≤0.4。
For second goal of the invention of the present invention, by mixing ytterbium oxide in PZT base piezoelectric ceramics so that in doping In the presence of element, Yb3+Into A or B positions, under 850~950 °C of sintering temperature, prepare and have good piezoelectric property concurrently PZT base piezoelectric ceramics, concrete technology step is as follows：
(1) preparation of PZT based ceramic powders body
According to formulaxPb(Ni1/3Nb2/3)O3–yPb(Mg1/2W1/2)O3–(1–x–y)Pb(Zr0.3Ti0.7)O3+u wt% Ba(W1/ 2Cu1/2)+v mol% Yb2O3Represent, 0.1≤x≤0.8,0.02≤y≤0.15, 0.01≤ u ≤0.5, 0≤v≤ 0.4, Calculate and weigh each raw material, by each raw material after ball mill crushing and mix homogeneously, 2 ~ 4 h, insulation are incubated under 750 ~ 850 °C Room temperature and again ball mill crushing are cooled to after end, PZT based ceramic powder bodies are obtained；
(2) pelletize tabletting
To step（1）The poly-vinyl alcohol solution of 5 ~ 10 wt% is added to carry out pelletize in gained PZT based ceramic powder bodies, then by gained Pellet is tabletted, obtains PZT base potsherds；
(3) dumping sintering
By step（2）In 850 ~ 950 °C of h of lower heat preservation sintering 2 ~ 4 after gained PZT base potsherd dumpings, obtain sintering PZT base pressures Electroceramics piece；
(4) polarize
By step（3）Gained obtains sintering after the silver paste that PZT base piezoelectric ceramics disk surfaces coat 5 ~ 15 wt%, 650 ~ 750 °C min of lower heat preservation sintering 10 ~ 20, insulation is cooled to room temperature after terminating, and is then polarized in silicone oil, obtains ytterbium oxide and mixes Miscellaneous PZT piezoelectric ceramics.
In said method, step（1）In the concrete technology of ball milling twice be preferably：With dehydrated alcohol as disperse medium, press It is 1 according to the mass ratio of each raw material total amount and dehydrated alcohol:1.5 add each raw material and dehydrated alcohol in ball grinder, celestial body of being expert at With the h of rotating speed ball milling 10 ~ 24 of 100 ~ 450 rmp on grinding machine, it is dried after ball milling.The drying can be dried under heat lamp It is roasting 2 ~ 3 hours.
In said method, the tabletted concrete technology of gained pellet is preferably：Push in the pressure of 10 ~ 20 MPa Make diameter and be about 10 ~ 15 mm, thickness is about the PZT base piezoelectric ceramic pieces of the ytterbium oxide doping of 0.8 ~ 1.2 mm.
In said method, step（2）Described in poly-vinyl alcohol solution concentration be preferably 5 ~ 10 wt%.
In said method, the concrete technology of dumping is preferably in step (3)：By step（2）Gained PZT base potsherds exist 4 ~ 10 h are incubated under 450 ~ 550 °C.
In said method, step（4）In the concrete technology that polarized in silicone oil be：In 60 ~ 120 °C of silicone oil, Polarization field strength is that the min of electric field intensity 15 ~ 30 is kept under the conditions of 2 ~ 5 kV/mm.
Compared with prior art, the invention has the advantages that：
1st, the ytterbium oxide doped PZT base piezoelectric ceramic that the present invention is provided, sintering temperature is low, is 850~950 °C and with good Piezoelectric property,d 33Up to 608 pC/N, are measured at room temperature using Agilent 4294A precise impedance instrument under the frequency of 1 kHz Dielectric loss is not more than 3/1000ths, and Curie temperature is more than 170 DEG C, as shown in Figure 4.
2nd, the ytterbium oxide doped PZT base piezoelectric ceramic that the present invention is provided, its thing is mutually pure perovskite phase, as shown in figure 1, mixing Ytterbium oxide doping improves sintering activity and makes crystal grain dense uniform and grow abundant, densification.
Description of the drawings
Fig. 1 is the X-ray diffraction of the piezoceramic material that embodiment 1~6 is prepared（XRD）Collection of illustrative plates.
Fig. 2 is the piezoelectric property figure of the piezoceramic material that embodiment 1~6 is prepared.
Fig. 3 is the change of the dielectric constant with temperature of the piezoceramic material that embodiment 1~6 is prepared.
Fig. 4 is the electro-acoustic element schematic diagram of the piezoceramic material that embodiment 2 is prepared.
Specific embodiment
The PZT base piezoelectric ceramics adulterated to ytterbium oxide of the present invention below by specific embodiment are made furtherly It is bright.
Embodiment 1
(1) preparation of PZT based ceramic powders body
According to logical 0.4Pb (Ni1/3Nb2/3)O3-0.02Pb(Mg1/2W1/2)O3–0.58Pb(Zr0.3Ti0.7)O3+0.05wt% Ba (W1/2Cu1/2)+0 mol% Yb2O3Represent,（x=0.4, y=0.02, u=0.05, v=0）Calculate and weigh each raw material, with anhydrous second Alcohol is disperse medium, is 1 according to the mass ratio of each raw material total amount and dehydrated alcohol:Each raw material and dehydrated alcohol are added goal by 1.5 In grinding jar, with the h of rotating speed ball milling 24 of 100 rmp on planetary ball mill, baking is dried for 2 hours under heat lamp after ball milling To mixed powder, gained mixed powder is incubated into 3h under 800 °C, insulation is cooled to room temperature and again according to identical after terminating Method carries out second ball milling, and baking is dried for 3 hours under heat lamp after ball milling, obtains PZT based ceramic powder bodies；
(2) pelletize tabletting
To step（1）The poly-vinyl alcohol solution that concentration is 10 wt% is added to carry out pelletize, Ran Hou in gained PZT based ceramic powder bodies Diameter is pressed under the pressure of 10 MPa and is about 10mm, thickness is about the PZT base piezoelectric ceramic disks of 1.2 mm；
(3) dumping sintering
By step（2）Gained PZT bases potsherd is incubated after 4 h carry out dumping under 550 °C, in 850 °C of lower heat preservation sinterings 4 H, obtains sintering PZT base piezoelectric ceramic pieces；
(4) polarize
By step（3）Gained sintering PZT base piezoelectric ceramics disk surfaces are coated after the silver paste of 10 wt%, and the insulation under 650 °C is burnt 20 min are tied, insulation is cooled to room temperature after terminating, then in 60 °C of silicone oil, Polarization field strength is to protect under the conditions of 5 kV/mm Hold the min of electric field intensity 15 to be polarized, obtain the PZT piezoelectric ceramics of ytterbium oxide doping.
The XRD spectrum of the PZT piezoelectric ceramics of obtained ytterbium oxide doping is shown in that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is pure calcium Titanium ore phase；Using Chinese Academy of Sciences's acoustics ZJ-3 type quasistaticsd 33Instrument, the piezoelectric moduluses for measuringd 33See Fig. 3, be 322 pC/ N；Connect the change that temperature controlling stove measures dielectric constant with temperature using Agilent 4980A precise impedance instrument, sample can be obtained from Fig. 4 Curie temperature be 171 °C.
Embodiment 2
(1) preparation of PZT based ceramic powders body
According to formula 0.42Pb (Ni1/3Nb2/3)O3-0.04Pb(Mg1/2W1/2)O3–0.54Pb(Zr0.3Ti0.7)O3+0.05wt% Ba (W1/2Cu1/2)+0.05 mol% Yb2O3Represent,（x=0.42, y=0.04, u=0.05, v=0.05）Calculate and weigh each raw material, It is 1 according to the mass ratio of each raw material total amount and dehydrated alcohol with dehydrated alcohol as disperse medium:1.5 by each raw material and anhydrous second Alcohol is added in ball grinder, and with the h of rotating speed ball milling 10 of 450 rmp on planetary ball mill, baking is entered for 3 hours under heat lamp after ball milling Row is dried to obtain mixed powder, and gained mixed powder is incubated into 4 h under 750 °C, and insulation is cooled to room temperature and again after terminating Second ball milling is carried out by the same way, and baking is dried for 3 hours under heat lamp after ball milling, obtains PZT based ceramic powder bodies；
(2) pelletize tabletting
To step（1）The poly-vinyl alcohol solution that concentration is 8 wt% is added to carry out pelletize, Ran Hou in gained PZT based ceramic powder bodies Diameter is pressed under the pressure of 20 MPa and is about 14 mm, thickness is about the PZT base piezoelectric ceramic disks of 0.9 mm；
(3) dumping sintering
By step（2）Gained PZT bases potsherd is incubated after 4 h carry out dumping under 550 °C, in 900 °C of lower heat preservation sinterings 3 H, obtains sintering PZT base piezoelectric ceramic pieces；
(4) polarize
By step（3）Gained sintering PZT base piezoelectric ceramics disk surfaces are coated after the silver paste of 12 wt%, and the insulation under 700 °C is burnt 10 min are tied, insulation is cooled to room temperature after terminating, then in 60 °C of silicone oil, Polarization field strength is to protect under the conditions of 2 kV/mm Hold the min of electric field intensity 30 to be polarized, obtain the PZT piezoelectric ceramics of ytterbium oxide doping.
The XRD spectrum of the PZT piezoelectric ceramics of obtained ytterbium oxide doping is shown in that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is pure calcium Titanium ore phase；Using Chinese Academy of Sciences's acoustics ZJ-3 type quasistaticsd 33Instrument, the piezoelectric moduluses for measuringd 33See Fig. 3, be 513 pC/ N；Connect the change that temperature controlling stove measures dielectric constant with temperature using Agilent 4980A precise impedance instrument, sample can be obtained from Fig. 4 Curie temperature be 178 °C.
Embodiment 3
(1) preparation of PZT based ceramic powders body
According to formula 0.44Pb (Ni1/3Nb2/3)O3-0.04Pb(Mg1/2W1/2)O3–0.52Pb(Zr0.3Ti0.7)O3+0.05wt% Ba (W1/2Cu1/2)+0.1 mol% Yb2O3Represent,（x=0.44, y=0.04, u=0.05, v=0.1）Calculate and weigh each raw material, with Dehydrated alcohol is disperse medium, is 1 according to the mass ratio of each raw material total amount and dehydrated alcohol:1.5 by each raw material and dehydrated alcohol In adding ball grinder, with the h of rotating speed ball milling 18 of 300 rmp on planetary ball mill, baking is carried out for 3 hours under heat lamp after ball milling Be dried to obtain mixed powder, gained mixed powder be incubated into 2 h under 850 °C, insulation be cooled to after terminating room temperature and again by Second ball milling is carried out according to same procedure, baking is dried for 2 hours under heat lamp after ball milling, obtains PZT based ceramic powder bodies；
(2) pelletize tabletting
To step（1）The poly-vinyl alcohol solution that concentration is 10 wt% is added to carry out pelletize, Ran Hou in gained PZT based ceramic powder bodies Diameter is pressed under the pressure of 15 MPa and is about 13 mm, thickness is about the PZT base piezoelectric ceramic disks of 1mm；
(3) dumping sintering
By step（2）Gained PZT bases potsherd is incubated after 10 h carry out dumping under 450 °C, in 950 °C of lower heat preservation sinterings 2h, obtains sintering PZT base piezoelectric ceramic pieces；
(4) polarize
By step（3）After the silver paste of gained sintering PZT base piezoelectric ceramics disk surfaces coating 5wt%, in 750 °C of lower heat preservation sinterings 10 min, insulation is cooled to room temperature after terminating, and then in 60 °C of silicone oil, Polarization field strength is to keep under the conditions of 4 kV/mm Electric field intensity 16min is polarized, and obtains the PZT piezoelectric ceramics of ytterbium oxide doping.
The XRD spectrum of the PZT piezoelectric ceramics of obtained ytterbium oxide doping is shown in that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is pure calcium Titanium ore phase；Using Chinese Academy of Sciences's acoustics ZJ-3 type quasistaticsd 33Instrument, the piezoelectric moduluses for measuringd 33See Fig. 3, be 608 pC/ N；Connect the change that temperature controlling stove measures dielectric constant with temperature using Agilent 4980A precise impedance instrument, sample can be obtained from Fig. 4 Curie temperature be 173 °C.Its SEM figure is shown in Fig. 2, shows its even grain size, and intercrystalline is comparatively dense.
Embodiment 4
(1) preparation of PZT based ceramic powders body
According to formula 0.46Pb (Ni1/3Nb2/3)O3-0.06Pb(Mg1/2W1/2)O3–0.48Pb(Zr0.3Ti0.7)O3+0.05wt% Ba (W1/2Cu1/2)+0.15 mol% Yb2O3Represent,（x=0.46, y=0.06, u=0.05, v=0.15）Calculate and weigh each raw material, It is 1 according to the mass ratio of each raw material total amount and dehydrated alcohol with dehydrated alcohol as disperse medium:1.5 by each raw material and anhydrous second Alcohol is added in ball grinder, and with the h of rotating speed ball milling 20 of 200 rmp on planetary ball mill, baking is entered for 3 hours under heat lamp after ball milling Row is dried to obtain mixed powder, and gained mixed powder is incubated into 3h under 800 °C, and insulation is cooled to room temperature and again after terminating Second ball milling is carried out by the same way, and baking is dried for 3 hours under heat lamp after ball milling, obtains PZT based ceramic powder bodies；
(2) pelletize tabletting
To step（1）The poly-vinyl alcohol solution that concentration is 10 wt% is added to carry out pelletize, Ran Hou in gained PZT based ceramic powder bodies Diameter is pressed under the pressure of 20 MPa and is about 15 mm, thickness is about the PZT base piezoelectric ceramic disks of 0.8mm；
(3) dumping sintering
By step（2）Gained PZT bases potsherd is incubated after 8 h carry out dumping under 500 °C, in 900 °C of lower heat preservation sinterings 4 H, obtains sintering PZT base piezoelectric ceramic pieces；
(4) polarize
By step（3）Gained sintering PZT base piezoelectric ceramics disk surfaces are coated after the silver paste of 15 wt%, and the insulation under 650 °C is burnt 15 min are tied, insulation is cooled to room temperature after terminating, then in 60 °C of silicone oil, Polarization field strength is to protect under the conditions of 5 kV/mm Hold the min of electric field intensity 25 to be polarized, obtain the PZT piezoelectric ceramics of ytterbium oxide doping.
The XRD spectrum of the PZT piezoelectric ceramics of obtained ytterbium oxide doping is shown in that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is pure calcium Titanium ore phase；Using Chinese Academy of Sciences's acoustics ZJ-3 type quasistaticsd 33Instrument, the piezoelectric moduluses for measuringd 33See Fig. 3, be 555 pC/ N；Connect the change that temperature controlling stove measures dielectric constant with temperature using Agilent 4980A precise impedance instrument, sample can be obtained from Fig. 4 Curie temperature be 177 °C.
Embodiment 5
(1) preparation of PZT based ceramic powders body
According to formula 0.48Pb (Ni1/3Nb2/3)O3-0.08Pb(Mg1/2W1/2)O3–0.44Pb(Zr0.3Ti0.7)O3+0.05 wt% Ba(W1/2Cu1/2)+0.2 mol% Yb2O3Represent,（x=0.48, y=0.08, u=0.05, v=0.2）Calculate and weigh each raw material, It is 1 according to the mass ratio of each raw material total amount and dehydrated alcohol with dehydrated alcohol as disperse medium:1.5 by each raw material and anhydrous second Alcohol is added in ball grinder, and with the h of rotating speed ball milling 11 of 400 rmp on planetary ball mill, baking is entered for 2 hours under heat lamp after ball milling Row is dried to obtain mixed powder, and gained mixed powder is incubated into 4 h under 750 °C, and insulation is cooled to room temperature and again after terminating Second ball milling is carried out by the same way, and baking is dried for 3 hours under heat lamp after ball milling, obtains PZT based ceramic powder bodies；
(2) pelletize tabletting
To step（1）The poly-vinyl alcohol solution that concentration is 6 wt% is added to carry out pelletize, Ran Hou in gained PZT based ceramic powder bodies Diameter is pressed under the pressure of 18 MPa and is about 10 mm, thickness is about the PZT base piezoelectric ceramic disks of 1.2 mm；
(3) dumping sintering
By step（2）Gained PZT bases potsherd is incubated under 500 °C after 7h carries out dumping, in 900 °C of h of lower heat preservation sintering 4, Obtain sintering PZT base piezoelectric ceramic pieces；
(4) polarize
By step（3）Gained sintering PZT base piezoelectric ceramics disk surfaces are coated after the silver paste of 10 wt%, and the insulation under 750 °C is burnt Knot 12min, insulation is cooled to room temperature after terminating, and then in 60 °C of silicone oil, Polarization field strength is to keep under the conditions of 3kV/mm The min of electric field intensity 30 is polarized, and obtains the PZT piezoelectric ceramics of ytterbium oxide doping.
The XRD spectrum of the PZT piezoelectric ceramics of obtained ytterbium oxide doping is shown in that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is pure calcium Titanium ore phase；Using Chinese Academy of Sciences's acoustics ZJ-3 type quasistaticsd 33Instrument, the piezoelectric moduluses for measuringd 33See Fig. 3, be 557pC/N； Connect the change that temperature controlling stove measures dielectric constant with temperature using Agilent 4980A precise impedance instrument, sample can be obtained from Fig. 4 Curie temperature is 175 °C.
Embodiment 6
(1) preparation of PZT based ceramic powders body
According to formula 0.50Pb (Ni1/3Nb2/3)O3-0.10Pb(Mg1/2W1/2)O3–0.40Pb(Zr0.3Ti0.7)O3+0.05wt% Ba (W1/2Cu1/2)+0.3 mol% Yb2O3Represent,（x=0.5, y=0.1, u=0.05, v=0.3）Calculate and weigh each raw material, with nothing Water-ethanol is disperse medium, is 1 according to the mass ratio of each raw material total amount and dehydrated alcohol:1.5 add each raw material and dehydrated alcohol In entering ball grinder, with the h of rotating speed ball milling 24 of 100 rmp on planetary ball mill, baking is done for 2 hours under heat lamp after ball milling It is dry to obtain mixed powder, gained mixed powder is incubated into 3h under 800 °C, insulation be cooled to after terminating room temperature and again according to Same procedure carries out second ball milling, and baking is dried for 3 hours under heat lamp after ball milling, obtains PZT based ceramic powder bodies；
(2) pelletize tabletting
To step（1）The poly-vinyl alcohol solution that concentration is 10 wt% is added to carry out pelletize, Ran Hou in gained PZT based ceramic powder bodies Diameter is pressed under the pressure of 10 MPa and is about 10mm, thickness is about the PZT base piezoelectric ceramic disks of 1.2 mm；
(3) dumping sintering
By step（2）Gained PZT bases potsherd is incubated after 4 h carry out dumping under 550 °C, in 850 °C of lower heat preservation sinterings 4 H, obtains sintering PZT base piezoelectric ceramic pieces；
(4) polarize
By step（3）Gained sintering PZT base piezoelectric ceramics disk surfaces are coated after the silver paste of 10 wt%, and the insulation under 650 °C is burnt 20 min are tied, insulation is cooled to room temperature after terminating, then in 60 °C of silicone oil, Polarization field strength is to protect under the conditions of 5 kV/mm Hold the min of electric field intensity 15 to be polarized, obtain the PZT piezoelectric ceramics of ytterbium oxide doping.
The XRD spectrum of the PZT piezoelectric ceramics of obtained ytterbium oxide doping is shown in that Fig. 1, Fig. 1 show that PZT piezoelectric ceramics is pure calcium Titanium ore phase；Using Chinese Academy of Sciences's acoustics ZJ-3 type quasistaticsd 33Instrument, the piezoelectric moduluses for measuringd 33See Fig. 3, be 509 pC/ N；Connect the change that temperature controlling stove measures dielectric constant with temperature using Agilent 4980A precise impedance instrument, sample can be obtained from Fig. 4 Curie temperature be 179 °C.
Embodiment 7
(1) preparation of PZT based ceramic powders body
According to formula 0.52Pb (Ni1/3Nb2/3)O3-0.10Pb(Mg1/2W1/2)O3–0.38Pb(Zr0.3Ti0.7)O3+0.05wt% Ba (W1/2Cu1/2)+0.1 mol% Yb2O3Represent,（x=0.52, y=0.10, u=0.05, v=0.1）Calculate and weigh each raw material, with Dehydrated alcohol is disperse medium, is 1 according to the mass ratio of each raw material total amount and dehydrated alcohol:1.5 by each raw material and dehydrated alcohol In adding ball grinder, with the h of rotating speed ball milling 24 of 100 rmp on planetary ball mill, baking is carried out for 2 hours under heat lamp after ball milling Be dried to obtain mixed powder, gained mixed powder be incubated into 3h under 800 °C, insulation be cooled to after terminating room temperature and again by Second ball milling is carried out according to same procedure, baking is dried for 3 hours under heat lamp after ball milling, obtains PZT based ceramic powder bodies；
(2) pelletize tabletting
To step（1）The poly-vinyl alcohol solution that concentration is 10 wt% is added to carry out pelletize, Ran Hou in gained PZT based ceramic powder bodies Diameter is pressed under the pressure of 10 MPa and is about 10mm, thickness is about the PZT base piezoelectric ceramic disks of 1.2 mm；
(3) dumping sintering
By step（2）Gained PZT bases potsherd is incubated after 4 h carry out dumping under 550 °C, in 850 °C of lower heat preservation sinterings 4 H, obtains sintering PZT base piezoelectric ceramic pieces；
(4) polarize
By step（3）Gained sintering PZT base piezoelectric ceramics disk surfaces are coated after the silver paste of 10 wt%, and the insulation under 650 °C is burnt 20 min are tied, insulation is cooled to room temperature after terminating, then in 60 °C of silicone oil, Polarization field strength is to protect under the conditions of 5 kV/mm Hold the min of electric field intensity 15 to be polarized, obtain the PZT piezoelectric ceramics of ytterbium oxide doping.
Embodiment 8
(1) preparation of PZT based ceramic powders body
According to formula 0.50Pb (Ni1/3Nb2/3)O3-0.08Pb(Mg1/2W1/2)O3–0.42Pb(Zr0.3Ti0.7)O3+0.05wt% Ba (W1/2Cu1/2)+0.3 mol% Yb2O3Represent,（x=0.5, y=0.08, u=0.05, v=0.1）Calculate and weigh each raw material, with nothing Water-ethanol is disperse medium, is 1 according to the mass ratio of each raw material total amount and dehydrated alcohol:1.5 add each raw material and dehydrated alcohol In entering ball grinder, with the h of rotating speed ball milling 24 of 100 rmp on planetary ball mill, baking is done for 2 hours under heat lamp after ball milling It is dry to obtain mixed powder, gained mixed powder is incubated into 3h under 800 °C, insulation be cooled to after terminating room temperature and again according to Same procedure carries out second ball milling, and baking is dried for 3 hours under heat lamp after ball milling, obtains PZT based ceramic powder bodies；
(2) pelletize tabletting
To step（1）The poly-vinyl alcohol solution that concentration is 10 wt% is added to carry out pelletize, Ran Hou in gained PZT based ceramic powder bodies Diameter is pressed under the pressure of 10 MPa and is about 10mm, thickness is about the PZT base piezoelectric ceramic disks of 1.2 mm；
(3) dumping sintering
By step（2）Gained PZT bases potsherd is incubated after 4 h carry out dumping under 550 °C, in 850 °C of lower heat preservation sinterings 4 H, obtains sintering PZT base piezoelectric ceramic pieces；
(4) polarize
By step（3）Gained sintering PZT base piezoelectric ceramics disk surfaces are coated after the silver paste of 10 wt%, and the insulation under 650 °C is burnt 20 min are tied, insulation is cooled to room temperature after terminating, then in 60 °C of silicone oil, Polarization field strength is to protect under the conditions of 5 kV/mm Hold the min of electric field intensity 15 to be polarized, obtain the PZT piezoelectric ceramics of ytterbium oxide doping
Application examples 1
The PZT based piezoelectric ceramic materials of the ytterbium oxide doping that embodiment 2 is prepared are prepared into 0.2 millimeter of thickness, diameter 12 The disk of millimeter, plus Top electrode, lead, diaphragm, shell etc. make electro-acoustic element, as shown in Figure 4.

Claims (10)

1. a kind of ytterbium oxide doped PZT base piezoelectric ceramic, it is characterised in that the chemical general formula of the piezoelectric ceramics isxPb(Ni1/ 3Nb2/3)O3– yPb(Mg1/2W1/2)O3– (1–x–y)Pb(Zr0.3Ti0.7)O3+ u wt% Ba(W1/2Cu1/2)+ v mol% Yb2O3, 0.1≤x≤ 0.8,0.02≤y≤0.15, 0.01≤u≤0.5, 0≤v≤0.4。
2. the preparation method of ytterbium oxide doped PZT base piezoelectric ceramic described in claim 1, it is characterised in that processing step is as follows：
(1) preparation of PZT based ceramic powders body
According to formulaxPb(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, calculates and weighs each raw material, by each raw material after ball mill crushing and mix homogeneously, under 750 ~ 850 °C 2 ~ 4 h of insulation, insulation is cooled to room temperature and again ball mill crushing, obtains PZT based ceramic powder bodies after terminating；
(2) pelletize tabletting
To step（1）Add poly-vinyl alcohol solution to carry out pelletize in gained PZT based ceramic powder bodies, be then pressed into gained pellet Piece, obtains PZT base potsherds；
(3) dumping sintering
By step（2）In 850 ~ 950 °C of h of lower heat preservation sintering 2 ~ 4 after gained PZT base potsherd dumpings, obtain sintering PZT base pressures Electroceramics piece；
(4) polarize
By step（3）Gained sintering PZT base piezoelectric ceramics disk surfaces are coated after the silver paste of 5 ~ 15 wt%, under 650 ~ 750 °C The min of heat preservation sintering 10 ~ 20, insulation is cooled to room temperature after terminating, and is then polarized in silicone oil, obtains ytterbium oxide doped PZT Base piezoelectric ceramic.
3. the preparation method of ytterbium oxide doped PZT base piezoelectric ceramic according to claim 2, it is characterised in that step（1）In Twice the concrete technology of ball milling is：With dehydrated alcohol as disperse medium, it is according to each raw material total amount and the mass ratio of dehydrated alcohol 1:1.5 add each raw material and dehydrated alcohol in ball grinder, on planetary ball mill with the rotating speed ball milling 10 of 100 ~ 450 rmp ~ 24 h, are dried after ball milling.
4. the preparation method of ytterbium oxide doped PZT base piezoelectric ceramic according to claim 3, it is characterised in that the drying is Toasting 2 ~ 3 hours under heat lamp.
5. according to any claim in claim 2 ~ 4 ytterbium oxide doped PZT base piezoelectric ceramic preparation method, it is special It is step to levy（2）The middle concrete technology that gained pellet is tabletted is：Diameter is pressed under the pressure of 10 ~ 20 MPa about For 10 ~ 15 mm, thickness is about the ytterbium oxide doped PZT base piezoelectric ceramic piece of 0.8 ~ 1.2 mm.
6. according to any claim in claim 2 ~ 4 ytterbium oxide doped PZT base piezoelectric ceramic preparation method, it is special It is step to levy（2）Described in poly-vinyl alcohol solution concentration be 5 ~ 10 wt%.
7. according to any claim in claim 2 ~ 4 ytterbium oxide doped PZT base piezoelectric ceramic preparation method, it is special It is step to levy（3）The concrete technology of middle dumping is：By step（2）Gained PZT bases potsherd is incubated 4 under 450 ~ 550 °C ~ 10 h。
8. according to any claim in claim 5 ytterbium oxide doped PZT base piezoelectric ceramic preparation method, its feature It is step（3）The concrete technology of middle dumping is：By step（2）Gained PZT bases potsherd is incubated 4 ~ 10 under 450 ~ 550 °C h。
9. according to any claim in claim 2 ~ 4 ytterbium oxide doped PZT base piezoelectric ceramic preparation method, it is special It is step to levy（4）In the concrete technology that polarized in silicone oil be：In 50 ~ 120 °C of silicone oil, Polarization field strength is 2 ~ 5 The min of electric field intensity 15 ~ 30 is kept under the conditions of kV/mm.
10. according to any claim in claim 5 ytterbium oxide doped PZT base piezoelectric ceramic preparation method, it is special It is step to levy（4）In the concrete technology that polarized in silicone oil be：In 50 ~ 120 °C of silicone oil, Polarization field strength is 2 ~ 5 The min of electric field intensity 15 ~ 30 is kept under the conditions of kV/mm.
CN201611176135.9A 2016-12-19 2016-12-19 Ytterbium oxide doped low-temperature prepared PZT (Piezoe-lectric Transducer) based piezoelectric ceramic Pending CN106673648A (en)

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CN109970090A (en) * 2019-05-14 2019-07-05 常州市卓群纳米新材料有限公司 The ultra-fine ytterbium oxide chemical preparation process that a kind of D50 is 1.5-2um
CN114573343A (en) * 2020-12-01 2022-06-03 四川大学 Low-temperature prepared high-performance PZT modified piezoelectric ceramic
CN114621007A (en) * 2020-12-14 2022-06-14 四川大学 Low-temperature prepared high-performance PZT-based multielement modified piezoelectric ceramic

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Publication number Priority date Publication date Assignee Title
CN107216130A (en) * 2017-06-06 2017-09-29 西安电子科技大学 A kind of preparation method of PHT PNN piezoceramic materials
CN107216130B (en) * 2017-06-06 2019-08-06 西安电子科技大学 A kind of preparation method of PHT-PNN piezoceramic material
CN109970090A (en) * 2019-05-14 2019-07-05 常州市卓群纳米新材料有限公司 The ultra-fine ytterbium oxide chemical preparation process that a kind of D50 is 1.5-2um
CN109970090B (en) * 2019-05-14 2021-06-25 常州市卓群纳米新材料有限公司 Chemical preparation method of superfine ytterbium oxide with D50 of 1.5-2um
CN114573343A (en) * 2020-12-01 2022-06-03 四川大学 Low-temperature prepared high-performance PZT modified piezoelectric ceramic
CN114621007A (en) * 2020-12-14 2022-06-14 四川大学 Low-temperature prepared high-performance PZT-based multielement modified piezoelectric ceramic
CN114621007B (en) * 2020-12-14 2023-06-23 四川大学 High-performance PZT-based multielement modified piezoelectric ceramic prepared at low temperature

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