CN102659404A - Plumbum niobate-nicklate (PNN)-plumbum zirconate titanate (PZT) piezoelectric ceramic capable of being sintered at low temperature and preparation method thereof - Google Patents
Plumbum niobate-nicklate (PNN)-plumbum zirconate titanate (PZT) piezoelectric ceramic capable of being sintered at low temperature and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a plumbum niobate-nicklate (PNN)-plumbum zirconate titanate (PZT) piezoelectric ceramic capable of being sintered at low temperature. The chemical formula of the PNN-PZT piezoelectric ceramic is 0.3Pb(Ni1/3Nb2/3)O3-0.7Pb(Zr0.44Ti0.56)O3+xCuO, wherein x is more than 0 and is less than or equal to 0.03. According to the PNN-PZT piezoelectric ceramic, a 0.3 PNN-0.7 PZT ternary piezoelectric ceramic material with high comprehensive performance is prepared by the conventional oxide mixing method and sintering CuO at low temperature under normal pressure on the basis of a Pb(Ni1/3Nb2/3)O3-Pb(Zr0.44Ti0.56)O3 system, so that the piezoelectric ceramic which can be sintered at low temperature and has high comprehensive performance is provided. The PNN-PZT piezoelectric ceramic is mainly applied to electronic devices of multilayer piezoelectric transformers, multilayer ceramic capacitors and the like which are sintered jointly at the low temperature.
Description
Technical field
The invention relates to the composition is the ceramic composition of characteristic, relates in particular to niobium nickel lead plumbate-Pb-based lanthanumdoped zirconate titanates (PNN-PZT) piezoelectric ceramics.
Background technology
Piezoelectric is the ceramic material that a kind of mechanical energy and electric energy transform each other, and it is a kind of material with piezoelectric property.Piezoelectric ceramics be a kind of can be with mechanical energy and the electric energy informational function stupalith of conversion mutually, piezoelectric ceramics also has dielectricity and elastic performance etc. except that having piezoelectric property.Piezoceramic material is owing to have excellent dielectricity and elastic performance, and preparation technology is simple, cost is low, therefore in high-technology field such as information, space flight, laser and biology and industrial production, has all obtained widespread use.
The PZT base piezoelectric ceramic is easily manufactured because of having, with low cost, electrical property is excellent, steady performance, and in production application, the lead base piezoelectric ceramics is still occupied an leading position.But traditional lead base sintering temperature of piezoelectric ceramics is higher, generally all about 1200 ℃～1300 ℃.Because the fusing point of PbO is very low, thereby inevitably causes PbO when high temperature sintering, seriously to volatilize.And the volatilization of PbO not only causes ceramic stoichiometric ratio to depart from the prescription of original design, makes its degradation; Also can work the mischief simultaneously the infringement human beings'health to environment.The volatilization of PbO when controlling high temperature sintering, sintering method commonly used at present mainly contains the sealing sintering process, buries burning method, atmosphere method, excess PbO method.But these methods can not fundamentally solve the volatilization of PbO, and only are to have guaranteed that the stoichiometric ratio in the prescription is constant.Therefore in order fundamentally to solve the PbO volatilization, actively and efficient ways is to realize the low-temperature sintering of piezoelectric ceramics.
Since nineteen nineties; Piezoelectric ceramic device is in order to adapt to the needs of integrated circuit surface package technique (SMT); Develop, and exploitation low-temperature melt piezoelectric ceramic (LTCC) material is the research direction of development high-performance, high reliability, low-cost ceramic laminated complex body to high-performance, microminiaturization, integrated, lightweight direction.The low-temperature melt piezoelectric ceramic main method has at present: add solubility promoter, chemical powdering method, pressure sintering and microwave sintering method.The recent development of piezo ceramic device is miniaturized, high stability and lower driving voltage, therefore needs the multi-layer piezoelectric device.The multi-layer piezoelectric device then inevitably need with ceramic co-fired metal inner electrode.Ag has the high and cheap advantage of specific conductivity and is widely used in the interior electrode of multi-layer piezoelectric device.General traditional lead base sintering temperature of piezoelectric ceramics very high (greatly about 1200 ℃), and the fusing point of Ag electrode is lower, is about 961 ℃, Ag or inner to pottery from electrode diffusion causes the unstable of multi-layered devices.On the other hand, in preparation laminated ceramic capacitor process, select for use pure Pd or Pd-Ag as interior electrode usually, cost is very high.Therefore, low-temperature melt piezoelectric ceramic has very important meaning, not only reduces energy consumption; Minimizing is to the harm of environment and human health; Can also reduce cost, select for use the relatively cheap metal of prices such as Ag, Cu, realize low temperature co-fired piezoelectric ceramics (LTCC) as interior electrode.
Many scholars had studied low-temperature sintering PNN-PZT piezoelectric ceramics, MgO, and NiO, ZnO, CuO etc. are good additives.Excessive N iO and PbO can reduce sintering temperature, obtain very high Kp at the PNN-PZT pottery of 900 ℃ of excessive NiO of following agglomerating.ZnO adds in the 0.41PNN-0.36PT-0.23PZ pottery, at 950 ℃ of sintering, very high dielectric and piezoelectric property is arranged.But, just very difficult at sintering below 950 ℃.And when CuO and ZnO co-doped 0.41PNN-0.36PT-0.23PZ, can be at 850 ℃ of following sintering.LiBiO
2Pb (Ni as sintering aid
1/3Nb
2/3) O
3-Pb (Zr
0.3Ti
0.7) O
3When being low to moderate 800 ℃, obtaining specific density is 97%, but and can promote grain growing.Sr doped P NZT-PNN piezoelectric ceramics can and obtain ferroelectric properties preferably at 900 ℃ of following sintering.CuO doping PMN-PZT piezoelectric ceramics can improve the sintering of pottery, can both be improved in lower temperature lower density and grain-size.During CuO doping PZT58-PNN piezoelectric ceramics, can make sintering temperature drop to 850 ℃ from 1200, in the sintering process, CuO and PbO reaction form liquid phase and have improved ceramic compactness.But because it too pursues low-temperature sintering when reducing sintering temperature, make the performance severe exacerbation on the contrary, this is fatal to piezoelectric ceramics.
Summary of the invention
The objective of the invention is; Solve the too high drawback of bringing of niobium nickel lead plumbate-Pb-based lanthanumdoped zirconate titanates (PNN-PZT) piezoelectric ceramics sintering temperature; Add CuO and reduce sintering temperature, a kind of ability low-temperature sintering is provided and can guarantees that it has niobium nickel lead plumbate-Pb-based lanthanumdoped zirconate titanates (PNN-PZT) piezoelectric ceramics of piezoelectric property preferably.
The present invention is achieved through following technical scheme.
Low-temperature sintering niobium nickel lead plumbate-lead titanate piezoelectric ceramics, its feed composition and mole percent level thereof are: 0.3Pb (Ni
1/3Nb
2/3) O
3-0.7Pb (Zr
0.44Ti
0.56) O
3+ xCuO, wherein 0＜x≤0.03.
Said raw material is Pb
3O
4, Ni
2O
3, Nb
2O
5, ZrO
2, TiO
2, CuO.
Its optimum material component and mole percent level thereof are 0.3Pb (Ni
1/3Nb
2/3) O
3-0.7Pb (Zr
0.44Ti
0.56) O
3+ xCuO, wherein x is 0.01.
Said piezoelectric ceramics is single calcium titanium ore structure.
The preparation method of low-temperature sintering niobium nickel lead plumbate-lead titanate piezoelectric ceramics has following steps:
(1) batching
With raw material Pb
3O
4, Ni
2O
3, Nb
2O
5, ZrO
2, TiO
2, CuO presses 0.3Pb (Ni
1/3Nb
2/3) O
3-0.7Pb (Zr
0.44Ti
0.56) 0
3+ xCuO, wherein the stoichiometric ratio of 0＜x≤0.03 is put into ball grinder after the mixing, and ball-milling medium is water and agate ball; Ball: material: the weight ratio of water is 2: 1: 0.6, and ball milling 4h, rotating speed are 750 rev/mins; Compound is put into 80 ℃ of oven dry of baking oven, put into mortar again and grind, cross 40 mesh sieves;
(2) synthetic
The powder that step (1) is ground after sieving is put into crucible, and compacting is added a cover, sealing, and 900 ℃ are synthesized in retort furnace, and insulation 2h naturally cools to room temperature, comes out of the stove;
(3) compressing tablet
With the synthetic material secondary ball milling of step (2), dry, sieve, the polyvinyl alcohol water solution that adds 5wt%～7wt% carries out granulation, afterwards it is smashed to pieces, presses down at the pressure of 250Mpa and processes diameter 12mm, thickness is the disk shape blank of 1.2mm;
(4) binder removal
Step (3) blank is put into retort furnace, respectively be incubated 0.5h in 200 ℃ and 350 ℃, temperature rise rate is 5 ℃/minute, to 650 ℃ of insulation 1h, carries out organism and gets rid of;
(5) sintering
Blank behind step (4) binder removal is put into crucible, seal, do to bury with similar powder and expect to bury burning, temperature rise rate is 6 ℃/minute, and in 900～1100 ℃ of sintering, insulation 2h naturally cools to room temperature with stove;
(6) silver ink firing
The ceramic plate that step (5) is sintered polish to thickness be 1.0mm, adopt screen printing technique lower surface printed silver slurry above that, place stove, be warming up to 750 ℃ and be incubated 10min, naturally cool to room temperature;
(7) polarization
Place silicone oil to be heated to 110～120 ℃ in the sample behind step (6) silver ink firing, apply the DC electric field of 2kv/mm, continue 10min, process piezoelectric ceramics;
(8) test piezoelectric property
With the piezoelectric ceramic piece after step (7) polarization, its piezoelectric property of test after leaving standstill 24h under the room temperature.
The preferred sintering temperature of said step (5) is 1050 ℃.
The invention has the beneficial effects as follows, with niobium nickel lead plumbate-Pb (Ni of Pb-based lanthanumdoped zirconate titanates system
1/3Nb
2/3) O
3-Pb (Zr
0.44Ti
0.56) O
3Be the basis; Adopt to add CuO and reduce the method for sintering temperature, the adjustment through prescription and technology and improve and prepare the 0.3PNN-0.7PZT ternary piezoceramic material with better over-all properties has reduced sintering temperature; Obtained a kind of piezoelectric ceramics of good combination property, wherein d
33=341pC/N, ε r=1986, tan δ=1.32%.
Embodiment
The raw material Pb that the present invention adopts
3O
4, Ni
2O
3, Nb
2O
5, ZrO
2, TiO
2And CuO, be commercially available CP raw material (purity>=99%).
Preparing method of the present invention is following:
(1) batching
With raw material Pb
3O
4, Ni
2O
3, Nb
2O
5, ZrO
2, TiO
2, CuO presses 0.3Pb (Ni
1/3Nb
2/3) O
3-0.7Pb (Zr
0.44Ti
0.56) O
3+ xCuO, wherein the stoichiometric ratio of 0＜x≤0.03 is put into ball grinder after the mixing, and ball-milling medium is water and agate ball; Ball: material: the weight ratio of water is 2: 1: 0.6, and ball milling 4h, rotating speed are 750 rev/mins; Compound is put into 80 ℃ of oven dry of baking oven, put into mortar again and grind, cross 40 mesh sieves;
(2) synthetic
The powder that step (1) is ground after sieving is put into crucible, and compacting is added a cover, sealing, and 900 ℃ are synthesized in retort furnace, and insulation 2h naturally cools to room temperature, comes out of the stove;
(3) compressing tablet
With the synthetic material secondary ball milling of step (2), dry, sieve, the polyvinyl alcohol water solution that adds 5wt%～7wt% carries out granulation, afterwards it is smashed to pieces, presses down at the pressure of 250Mpa and processes diameter 12mm, thickness is the disk shape blank of 1.2mm;
(4) binder removal
Step (3) blank is put into retort furnace, respectively be incubated 0.5h in 200 ℃ and 350 ℃, temperature rise rate is 5 ℃/minute, to 650 ℃ of insulation 1h, carries out organism and gets rid of;
(5) sintering
Blank behind step (4) binder removal is put into crucible, seal, do to bury with similar powder and expect to bury burning, temperature rise rate is 6 ℃/minute, and in 900～1100 ℃ of sintering, insulation 2h naturally cools to room temperature with stove;
(6) silver ink firing
It is the sample of 1.0mm that the ceramic plate that step (5) is sintered is polished to thickness, adopts screen printing technique lower surface printed silver slurry above that, places stove, is warming up to 750 ℃ and be incubated 10min, naturally cools to room temperature;
(7) polarization
Place silicone oil to be heated to 110～120 ℃ in the sample behind step (6) silver ink firing, apply the DC electric field of 2kv/mm, continue 10min, process piezoelectric ceramics;
(8) test piezoelectric property
With the piezoelectric ceramic piece after step (7) polarization, its piezoelectric property of test after leaving standstill 24h under the room temperature.
Specific embodiment is following:
X=0.01, sintering temperature is 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, is designated as embodiment 1-1,1-2,1-3,1-4,1-5 respectively
X=0.02, sintering temperature is 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, is designated as embodiment 2-1,2-2,2-3,2-4,2-5 respectively;
X=0.03, sintering temperature is 900 ℃, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, is designated as embodiment 3-1,3-2,3-3,3-4,3-5 respectively;
The piezoelectric and dielectric properties test result of the foregoing description is listed in table 1.
Table 1
When x=0.01, when sintering temperature is 1050 ℃ (embodiment 2-4), tan δ=1.32 * 10
-2(Automatic LCR Meter4225),
d
33=341PC/N (the quasistatic method, Model/ZJ-3A, China).
The piezoceramic material of the present invention's preparation is mainly used in the LTCC ceramic component low temperature co-fired with base-metal inner-electrode, like devices such as multilayer piezoelectric ceramic driving mechanism, multi-layer piezoelectric transformers.
Above-mentioned description to embodiment is to be convenient to the those of ordinary skill of this technical field can understand and use the present invention.The personnel of skilled obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (6)
1. low-temperature sintering niobium nickel lead plumbate-lead titanate piezoelectric ceramics, its feed composition and mole percent level thereof are: 0.3Pb (Ni
1/3Nb
2/3) O
3-0.7Pb (Zr
0.44Ti
0.56) O
3+ xCuO, wherein 0＜x≤0.03.
2. according to the low-temperature sintering niobium nickel lead plumbate-lead titanate piezoelectric ceramics of claim 1, it is characterized in that said raw material is Pb
3O
4, Ni
2O
3, Nb
2O
5, ZrO
2, TiO
2, CuO.
3. according to the low-temperature sintering niobium nickel lead plumbate-lead titanate piezoelectric ceramics of claim 1, it is characterized in that its optimum material component and mole percent level thereof are 0.3Pb (Ni
1/3Nb
2/3) O
3-0.7Pb (Zr
0.44Ti
0.56) O
3+ xCuO, wherein x is 0.01.
4. according to the low-temperature sintering niobium nickel lead plumbate-lead titanate piezoelectric ceramics of claim 1, it is characterized in that said piezoelectric ceramics is single calcium titanium ore structure.
5. the preparation method of the low-temperature sintering niobium nickel lead plumbate-lead titanate piezoelectric ceramics of claim 1 has following steps:
(1) batching
With raw material Pb
3O
4, Ni
2O
3, Nb
2O
5, ZrO
2, TiO
2, CuO presses 0.3Pb (Ni
1/3Nb
2/3) O
3-0.7Pb (Zr
0.44Ti
0.56) O
3+ xCuO, wherein the stoichiometric ratio of 0＜x≤0.03 is put into ball grinder after the mixing, and ball-milling medium is water and agate ball; Ball: material: the weight ratio of water is 2: 1: 0.6, and ball milling 4h, rotating speed are 750 rev/mins; Compound is put into 80 ℃ of oven dry of baking oven, put into mortar again and grind, cross 40 mesh sieves;
(2) synthetic
The powder that step (1) is ground after sieving is put into crucible, and compacting is added a cover, sealing, and 900 ℃ are synthesized in retort furnace, and insulation 2h naturally cools to room temperature, comes out of the stove;
(3) compressing tablet
With the synthetic material secondary ball milling of step (2), dry, sieve, the polyvinyl alcohol water solution that adds 5wt%～7wt% carries out granulation, afterwards it is smashed to pieces, presses down at the pressure of 250Mpa and processes diameter 12mm, thickness is the disk shape blank of 1.2mm;
(4) binder removal
Step (3) blank is put into retort furnace, respectively be incubated 0.5h in 200 ℃ and 350 ℃, temperature rise rate is 5 ℃/minute, to 650 ℃ of insulation 1h, carries out organism and gets rid of;
(5) sintering
Blank behind step (4) binder removal is put into crucible, seal, do to bury with similar powder and expect to bury burning, temperature rise rate is 6 ℃/minute, and in 900～1100 ℃ of sintering, insulation 2h naturally cools to room temperature with stove;
(6) silver ink firing
The ceramic plate that step (5) is sintered polish to thickness be 1.0mm, adopt screen printing technique lower surface printed silver slurry above that, place stove, be warming up to 750 ℃ and be incubated 10min, naturally cool to room temperature;
(7) polarization
Place silicone oil to be heated to 110～120 ℃ in the sample behind step (6) silver ink firing, apply the DC electric field of 2kv/mm, continue 10min, process piezoelectric ceramics.
(8) test piezoelectric property
With the piezoelectric ceramic piece after step (7) polarization, its piezoelectric property of test after leaving standstill 24h under the room temperature.
6. according to the preparation method of the low-temperature sintering niobium nickel lead plumbate-lead titanate piezoelectric ceramics of claim 5, it is characterized in that the preferred sintering temperature of said step (5) is 1050 ℃.
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| CN102826846A (en) * | 2012-09-18 | 2012-12-19 | 天津大学 | Preparation method of high-performance aluminum oxide substrate lead niobate nickelate-lead zirconate titanate piezoelectric film |
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| 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 |
| CN108002832A (en) * | 2017-12-13 | 2018-05-08 | 中国振华(集团)新云电子元器件有限责任公司(国营第四三二六厂) | A kind of low temperature co-fired piezoceramic material and preparation method thereof |
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| CN102826846A (en) * | 2012-09-18 | 2012-12-19 | 天津大学 | Preparation method of high-performance aluminum oxide substrate lead niobate nickelate-lead zirconate titanate piezoelectric film |
| CN103214240A (en) * | 2013-03-20 | 2013-07-24 | 瑞声精密制造科技(常州)有限公司 | Piezoceramic material, sintered body, preparation method thereof, and piezoceramic device |
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