CN105355777A - Method for preparing PNN-PZN-PZT multi-layer parallel piezoelectric thick film on aluminium oxide substrate - Google Patents
Method for preparing PNN-PZN-PZT multi-layer parallel piezoelectric thick film on aluminium oxide substrate Download PDFInfo
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- CN105355777A CN105355777A CN201510688382.6A CN201510688382A CN105355777A CN 105355777 A CN105355777 A CN 105355777A CN 201510688382 A CN201510688382 A CN 201510688382A CN 105355777 A CN105355777 A CN 105355777A
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- 239000000758 substrate Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 238000007639 printing Methods 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims description 20
- 238000009413 insulation Methods 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000003786 synthesis reaction Methods 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- 230000010287 polarization Effects 0.000 claims description 5
- 230000005684 electric field Effects 0.000 claims description 4
- 239000001856 Ethyl cellulose Substances 0.000 claims description 3
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical group OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 229920001249 ethyl cellulose Polymers 0.000 claims description 3
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000011056 performance test Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000006073 displacement reaction Methods 0.000 abstract description 7
- 238000010344 co-firing Methods 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 30
- 239000000919 ceramic Substances 0.000 description 11
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 9
- 239000010955 niobium Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- NBJYBMGLGHPGGH-UHFFFAOYSA-N [Pb].[Ni].[Nb].[Zn].[Nb] Chemical compound [Pb].[Ni].[Nb].[Zn].[Nb] NBJYBMGLGHPGGH-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000002102 hyperpolarization Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 102220170006 rs886048021 Human genes 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/80—Constructional details
- H10N30/85—Piezoelectric or electrostrictive active materials
- H10N30/853—Ceramic compositions
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N30/00—Piezoelectric or electrostrictive devices
- H10N30/01—Manufacture or treatment
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- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a method for preparing a PNN-PZN-PZT multi-layer parallel piezoelectric thick film on an aluminium oxide substrate. The specific formula of the PNN-PZN-PZT multi-layer parallel piezoelectric thick film on the aluminium oxide substrate is 0.7Pb(ZryTi1-y)O3-zPb(Zn1/3Nb2/3)O3-(0.3-z)Pb(Ni1/3Nb2/3)O3. The method comprises the following steps: weighing and ball grinding raw materials according to the stoichiometric ratio of the above formula; presintering and synthesizing at 850 DEG C; printing electrodes and piezoelectric thick film layers by using a silk screen print method, wherein the piezoelectric thick film layers and the electrodes are overlapped alternately; and adjusting the low-temperature co-firing process to prepare the high-performance multi-layer parallel piezoelectric thick film material. The prepared PNN-PZN-PZT multi-layer parallel piezoelectric thick film is simple in process, low in cost, suitable for large-scale production, can be used for obtaining large drive force and displacement under a low voltage and is mainly applicable to a minidriver, an ultrasonic transducer and the like.
Description
Technical field
The invention belongs to a kind of take composition as the ceramic composition of feature, and particularly one prepares the method for PNN-PZN-PZT (niobium zinc-niobium nickel-lead zirconate titanate) Multi-layer Parallel piezoelectric thick on Al2O3 substrate.
Background technology
LTCC (LowTemperatureCo-firedCeramic, be called for short LTCC) be interconnected, the passive component of collection and encapsulation and multi-layer ceramics manufacturing technology integrally, it adopts thick-film material, according to the structure designed in advance, electrode material, substrate, electronic device etc. are burnt altogether below 900 DEG C, thus makes modularization integrated device or three-dimensional ceramic base multilayer circuit.Improving constantly in recent years along with the requirement to High-power piezoelectric material and device, the future development that piezoelectric ceramic devices are little to volume, driving voltage is low, displacement is large, energy is integrated, the research of low temperature co-fired multilayer piezoelectric ceramic becomes focus.
Piezoelectric ceramic piece is often bonded to multilayer piezoelectric ceramic with binding agent by traditional PZT ceramic component, due to the restriction by layered ceramic thickness, miniaturization, integrated cannot be realized, binding agent in multilayer components and parts is combined not tight with potsherd, easily separatedly cause penalty, even there is fracture, cannot Long-Time Service.But, no longer needing adhesive bond by being directly combined with interior electrode between ltcc layer, greatly improving in conjunction with compactness, the lamination between ceramic layer is overcome effectively, greatly increase the useful life of device, the croop property of device is also very significantly improved.In addition, low-temperature sintering can avoid the volatilization of PbO and the use of noble metal electrode effectively, reduces energy consumption, alleviates environmental pollution, product cost is reduced.In sum, low temperature co-fired multilayer piezoelectric ceramic has the advantage that volume is little, integration is high, operating voltage is low, the response time is short, displacement is large, is widely used in the preparation of the device such as lamination step transformer and stacked piezoelectric pottery micro positioner.
One of conventional preparation method of Multi-layer Parallel piezoelectric thick is silk screen print method, it is compared with additive method (the tape casting, hydro thermal method, sol-gal process), have with MEMS technology completely compatible, thickness can control and appropriate thickness, equipment is simple, raw material is cheap, cost is lower, gained piezoelectric thick density is high, is suitable for producing in enormous quantities, the advantage of favorable repeatability.But the thick film compactness prepared due to silk screen print method is poor, and the porosity is higher, and the performance of single layer thick film is lower, constrains its application.Multi-layer Parallel piezoelectric thick performance is that the number of plies is doubly linear to be increased, and efficiently solves the problem of single layer thick film poor-performing.
Summary of the invention
Object of the present invention, the shortcoming be that piezoelectric thick compactness prepared by the silk screen print method overcoming prior art is poor, the porosity is higher, the performance of single layer thick film is lower, restricting its application, provides a kind of at Al
2o
3the method of PNN-PZN-PZT Multi-layer Parallel piezoelectric thick prepared by substrate, to obtain the piezoelectric of high piezoelectric constant, Large strain, low driving voltage under less thickness; Adopt silver slurry as electrode material in addition, effectively reduce production cost.
The present invention is achieved by following technical solution:
A preparation method for PNN-PZN-PZT Multi-layer Parallel piezoelectric thick on aluminum oxide substrate, has following steps:
(1) prepare burden
By raw material Pb
3o
4, ZrO
2, TiO
2, Nb
2o
5, Ni
2o
30.7Pb (Zr is pressed with ZnO
0.46ti
0.54) O
3-0.1Pb (Zn
1/3nb
2/3) O
3-0.2Pb (Ni
1/3nb
2/3) O
3stoichiometric proportion batching, ball milling 4h, then dry in baking oven, sieves for subsequent use after grinding;
(2) synthesize
The powder of preparation in step (1) is put into crucible and compacting, adds a cover with zirconium powder sealing, in 850 DEG C of synthesis, insulation 2h;
(3) secondary ball milling
The synthesis material of step (2) is put into ball grinder, secondary ball milling 4 ~ 10h, then put into baking oven and dry, after drying, grinding is for subsequent use;
(4) frit is prepared
By raw material Pb
3o
4, H
3bO
3, SiO
2, Al
2o
3prepare burden according to the weight ratio of 15:2:7:1, put into ball grinder, ball milling 4h, then dry, grinding, sieves for subsequent use;
(5) piezoelectric thick slurry is prepared
Take the powder after the secondary ball milling of step (3), add the frit of step (4) and the organic carrier of 10wt.% of 1wt.%, mixed grinding makes slurry become thick and has certain mobility, reaches the state being applicable to printing; The mixed solution of described organic carrier to be triethanolamine, ethyl cellulose and terpinol be 1:4:45 weight ratio;
(6) thick film and electrode is printed
With distilled water by Al
2o
3substrate ultrasonic cleaning post-drying, adopts silk screen print method at Al
2o
3substrate prints electrode successively, piezoelectric thick layer; Repeat print electrode and piezoelectric thick layer, alternately laminated until complete 3 ~ 11 layers of parallel-connection structure, the first floor and most last layer are all electrode; Often printing one deck piezoelectric thick layer or electrode all in 120 DEG C of dry 10min, and then will continue printing;
(7) binder removal and sintering
The piezoelectric thick sample that step (6) prints is fired, rises to 800 ~ 900 DEG C, insulation 60 ~ 90min, with stove cooling, obtained PNN-PZN-PZT Multi-layer Parallel piezoelectric thick sample;
(8) polarize
The piezoelectric thick sample of step (7) is placed in the silicone oil of 140 DEG C, with the direct voltage of 6kV/mm polarization 10 ~ 15min, keeps electric field strength, stop heating, make it naturally cool to room temperature;
(9) performance test
By the piezoelectric thick sample of step (8) after polarization in left at room temperature 24h, measure piezoelectricity and dielectric property.
The raw material Pb of described step (1)
3o
4, ZrO
2, TiO
2, Nb
2o
5, Ni
2o
3and ZnO, be the chemical pure raw material of commercially available purity>=99%.
The ball-milling medium of described step (1) or step (3) or step (3) is deionized water and zirconia ball, ball: material: the weight ratio of water is 2:1:0.5; The rotating speed of ball mill is 750r/min.
The sintering schedule of described step (7) is: rise to 200 DEG C from room temperature 1.5 DEG C/min, insulation 30min; 250 DEG C are risen to again, insulation 40min with 1.5 DEG C/min; 400 DEG C are risen to again, insulation 60min with 1.5 DEG C/min; 800 ~ 900 DEG C are risen to again, insulation 60 ~ 90min with 3 DEG C/min; Cool with stove.
Beneficial effect of the present invention is as follows
1. production cost is low, and adopt screen printing technique and Ag electrode, sintering temperature is only 900 DEG C, far below the sintering temperature of conventional piezoelectric pottery, is conducive to large-scale industrial production.
2. at Al
2o
3substrate obtains smooth and high performance Multi-layer Parallel piezoelectric thick material.The performance of five layers of sample is: d
33=1021pC/N, ε
33 t/ ε
0=1167, tan δ=1.92%, P
r=56.44 μ C/cm
2.Eleventh floor properties of sample is: d
33=1835pC/N, ε
33 t/ ε
0=1003, tan δ=2.6%, P
r=86.776 μ C/cm
2, S33=0.66%.And in theory, the number of plies in parallel is more, piezoelectric property is better.
3. compared with piezoelectricity block materials, Multi-layer Parallel piezoelectric thick greatly reduces driving voltage, can obtain larger actuating force and displacement at the lower voltage.
Accompanying drawing explanation
Fig. 1 is five layers of parallel piezoelectric bulk structure schematic diagram of the embodiment of the present invention 1;
Fig. 2 is the surperficial sem analysis figure of the embodiment of the present invention 1;
Fig. 3 is section SEM and the EDX analysis chart of the embodiment of the present invention 2;
Fig. 4 is voltage-strain and the voltage-displacement curve figure of the embodiment of the present invention 2.
Embodiment
The raw materials used Pb of the present invention
3o
4, ZrO
2, TiO
2, Nb
2o
5, Ni
2o
3and ZnO, be the chemical pure raw material of commercially available purity>=99%, adopt conventional solid sintering method, specific embodiment is as follows:
Embodiment 1
(1) prepare burden
By raw material Pb
3o
4, ZrO
2, TiO
2, Nb
2o
5, Ni
2o
30.7Pb (Zr is pressed with ZnO
0.46ti
0.54) O
3-0.1Pb (Zn
1/3nb
2/3) O
3-0.2Pb (Ni
1/3nb
2/3) O
3stoichiometric proportion batching, put into ball grinder, ball-milling medium is deionized water and zirconia ball, ball: material: the weight ratio of water is 2:1:0.5, Ball-milling Time 4h, rotating speed is 750r/min, after ball milling by compound in baking oven in 120 DEG C of oven dry, then put into mortar to grind, cross 40 mesh sieves for subsequent use;
(2) synthesize
Powder in step (1) is put into crucible and compacting, adds a cover with zirconium powder sealing, 850 DEG C of synthesis in Muffle furnace, insulation 2h;
(3) secondary ball milling
Synthesis material grinding in step (2) is put into ball grinder, secondary ball milling 10h, and rotating speed is 750r/min, then puts into baking oven in 120 DEG C of oven dry, and after drying, grinding is for subsequent use;
(4) frit is prepared
By raw material Pb
3o
4, H
3bO
3, SiO
2, Al
2o
3prepare burden according to the weight ratio of 15:2:7:1, put into ball grinder, Ball-milling Time 4h, rotating speed is 750r/min, after ball milling by compound in baking oven in 120 DEG C of oven dry, dry after grinding, cross 60 mesh sieves for subsequent use;
(5) piezoelectric thick slurry is prepared
Take the powder after the secondary ball milling in step (3), add the frit of step (4) and the organic carrier of 10wt.% of 1wt.%, in mortar, mixed grinding is mixed, and makes slurry become thick, and have certain mobility, reach the state being applicable to printing; Described organic carrier is triethanolamine: ethyl cellulose: terpinol weight ratio=1:4:45;
(6) thick film and electrode is printed
With distilled water by Al
2o
3substrate ultrasonic cleaning post-drying is for subsequent use, adopts silk screen print method at Al
2o
3substrate prints electrode successively, piezoelectric thick layer, repeat print piezoelectric thick layer and electrode, alternately laminatedly finally print top electrode until 5 layers of piezoelectric structure, often print one deck all will in the baking oven of 120 DEG C dry 10min, continue printing after oven dry again; The Multi-layer Parallel piezoelectric thick structure of the present embodiment is see Fig. 1;
(7) binder removal and sintering
The piezoelectric thick printed in step (6) is put into Muffle furnace fire, sintering schedule is: rise to 200 DEG C from room temperature 1.5 DEG C/min, insulation 30min; 250 DEG C are risen to again, insulation 40min with 1.5 DEG C/min; 400 DEG C are risen to again, insulation 60min with 1.5 DEG C/min; 900 DEG C are risen to again, insulation 90min with 3 DEG C/min; With stove cooling, obtained PNN-PZN-PZT Multi-layer Parallel piezoelectric thick.The surperficial SEM microscopic appearance of the present embodiment is see Fig. 2, and as can be seen from Figure, the grain size of thick film is 1-3 μm, and density is higher, there is certain pore.
(8) polarize
The PNN-PZN-PZT Multi-layer Parallel piezoelectric thick that step (7) is obtained is placed in the silicone oil of 140 DEG C, after the direct voltage of 6kV/mm polarization 10min, keeps electric field strength, stop heating, make it naturally cool to room temperature;
(9) performance test
By in step (8) through the goods of hyperpolarization after left at room temperature 24h, measure its piezoelectricity and dielectric property.
Embodiment 2
Embodiment 2 just alternately laminated quantity becomes 11 layers, other processing step and parameter completely the same.
The section SEM figure of embodiment 2 and EDX energy spectrum analysis are see Fig. 3.As can be seen from the figure, combine between piezoelectric thick and electrode closely, clear in structure.
The performance comparison of 11 layers of piezoelectric thick and block materials is see Fig. 4.4-(a) is electric field-strain curve, and under the condition applying identical electric field, the strain that 11 layers of piezoelectric thick produces is higher than block materials; 4-(b) is voltage-displacement curve, obtain identical displacement, and the driving voltage of 11 layers of piezoelectric thick needs will be far smaller than block materials.
The electrical performance testing result of the specific embodiment of the invention 1,2 is as shown in table 1.
When the number of plies is 3 layers, its piezoelectric property can be suitable with block materials, and when the number of plies increases, piezoelectric property is that the number of plies doubly increases, and the more performances of the number of plies are better in theory.
Table 1
Claims (4)
1. the preparation method of PNN-PZN-PZT Multi-layer Parallel piezoelectric thick on aluminum oxide substrate, has following steps:
(1) prepare burden
By raw material Pb
3o
4, ZrO
2, TiO
2, Nb
2o
5, Ni
2o
30.7Pb (Zr is pressed with ZnO
0.46ti
0.54) O
3-0.1Pb (Zn
1/3nb
2/3) O
3-0.2Pb (Ni
1/3nb
2/3) O
3stoichiometric proportion batching, ball milling 4h, then dry in baking oven, sieves for subsequent use after grinding;
(2) synthesize
The powder of preparation in step (1) is put into crucible and compacting, adds a cover with zirconium powder sealing, in 850 DEG C of synthesis, insulation 2h;
(3) secondary ball milling
The synthesis material of step (2) is put into ball grinder, secondary ball milling 4 ~ 10h, then put into baking oven and dry, after drying, grinding is for subsequent use;
(4) frit is prepared
By raw material Pb
3o
4, H
3bO
3, SiO
2, Al
2o
3prepare burden according to the weight ratio of 15:2:7:1, put into ball grinder, ball milling 4h, then dry, through grinding, sieve for subsequent use;
(5) piezoelectric thick slurry is prepared
Take the powder after the secondary ball milling of step (3), add the frit of step (4) and the organic carrier of 10wt.% of 1wt.%, mixed grinding makes slurry become thick and has certain mobility, reaches the state being applicable to printing; Described organic carrier is triethanolamine, ethyl cellulose and the terpinol mixed solution by 1:4:45 weight ratio;
(6) thick film and electrode is printed
With distilled water by Al
2o
3substrate ultrasonic cleaning post-drying, adopts silk screen print method at Al
2o
3substrate prints electrode successively, piezoelectric thick layer; Repeat print electrode and piezoelectric thick layer, alternately laminated until complete 3 ~ 11 layers of parallel-connection structure, the first floor and most last layer are all electrode; Often printing one deck piezoelectric thick layer or electrode all in 120 DEG C of dry 10min, and then will continue printing;
(7) binder removal and sintering
The piezoelectric thick goods that step (6) prints are fired, rises to 800 ~ 900 DEG C, insulation 60 ~ 90min, with stove cooling, obtained PNN-PZN-PZT Multi-layer Parallel piezoelectric thick goods;
(8) polarize
The piezoelectric thick goods of step (7) are placed in the silicone oil of 140 DEG C, with the direct voltage of 6kV/mm polarization 10 ~ 15min, keep electric field strength, stop heating, make it naturally cool to room temperature;
(9) performance test
By the piezoelectric thick goods of step (8) after polarization in left at room temperature 24h, measure piezoelectricity and dielectric property.
2. the preparation method of PNN-PZN-PZT Multi-layer Parallel piezoelectric thick on aluminum oxide substrate according to claim 1, is characterized in that, the raw material Pb of described step (1)
3o
4, ZrO
2, TiO
2, Nb
2o
5, Ni
2o
3and ZnO, be the chemical pure raw material of commercially available purity>=99%.
3. the preparation method of PNN-PZN-PZT Multi-layer Parallel piezoelectric thick on aluminum oxide substrate according to claim 1, it is characterized in that, the ball-milling medium of described step (1) or step (3) or step (3) is deionized water and zirconia ball, ball: material: the weight ratio of water is 2:1:0.5; The rotating speed of ball mill is 750r/min.
4. the preparation method of PNN-PZN-PZT Multi-layer Parallel piezoelectric thick on aluminum oxide substrate according to claim 1, it is characterized in that, the sintering schedule of described step (7) is: rise to 200 DEG C from room temperature 1.5 DEG C/min, insulation 30min; 250 DEG C are risen to again, insulation 40min with 1.5 DEG C/min; 400 DEG C are risen to again, insulation 60min with 1.5 DEG C/min; 800 ~ 900 DEG C are risen to again, insulation 60 ~ 90min with 3 DEG C/min; Cool with stove.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108358629A (en) * | 2018-01-27 | 2018-08-03 | 天津大学 | The preparation of low temperature co-fired self-supporting PZT bases multi-layer piezoelectric thick film |
| CN110045150A (en) * | 2019-05-13 | 2019-07-23 | 中国工程物理研究院电子工程研究所 | A kind of On-line self-diagnosis survey piezoelectric acceleration sensor |
| CN113013321A (en) * | 2021-02-07 | 2021-06-22 | 西安交通大学 | Preparation method of piezoelectric single crystal laminated driver |
| CN113904585A (en) * | 2021-08-27 | 2022-01-07 | 成都汇通西电电子有限公司 | Array actuator structure and preparation method thereof |
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| CN113013321A (en) * | 2021-02-07 | 2021-06-22 | 西安交通大学 | Preparation method of piezoelectric single crystal laminated driver |
| CN113904585A (en) * | 2021-08-27 | 2022-01-07 | 成都汇通西电电子有限公司 | Array actuator structure and preparation method thereof |
| CN113904585B (en) * | 2021-08-27 | 2022-10-14 | 成都汇通西电电子有限公司 | Array actuator structure and preparation method thereof |
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